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Sample records for quadrupole mass spectrometer

  1. Differentially pumped dual linear quadrupole ion trap mass spectrometer

    Science.gov (United States)

    Owen, Benjamin C.; Kenttamaa, Hilkka I.

    2015-10-20

    The present disclosure provides a new tandem mass spectrometer and methods of using the same for analyzing charged particles. The differentially pumped dual linear quadrupole ion trap mass spectrometer of the present disclose includes a combination of two linear quadrupole (LQIT) mass spectrometers with differentially pumped vacuum chambers.

  2. Differentially pumped dual linear quadrupole ion trap mass spectrometer

    Science.gov (United States)

    Owen, Benjamin C.; Kenttamaa, Hilkka I.

    2016-11-15

    The present disclosure provides a new tandem mass spectrometer and methods of using the same for analyzing charged particles. The differentially pumped dual linear quadrupole ion trap mass spectrometer of the present disclose includes a combination of two linear quadrupole (LQIT) mass spectrometers with differentially pumped vacuum chambers.

  3. Quadrupole Time-of-Flight Mass Spectrometer

    Data.gov (United States)

    Federal Laboratory Consortium — FUNCTION: The system generates superior quality mass spectrometry (MS) and tandem mass spectrometry (MS/MS) data from both atmospheric pressure ionization (API) and...

  4. Determining gaseous composition of fluid inclusions with quadrupole mass spectrometer

    Institute of Scientific and Technical Information of China (English)

    朱和平; 王莉娟

    2002-01-01

    Quadrupole mass spectrometer (QMS) is an instrument for effectively determining gaseous composition of fluid inclusion. The gaseous component is extracted from inclusions with thermal decrepitation method and then determined with the sensitive QMS instrument. The method is characterized by high sensitivity and high accuracy with the relative standard deviation (RSD, n = 6) of less than 3%. It has been successfully used for analyzing fluid inclusions. The analytical re-sults meet the requirement of geological study.

  5. Targeted proteomic quantification on quadrupole-orbitrap mass spectrometer.

    Science.gov (United States)

    Gallien, Sebastien; Duriez, Elodie; Crone, Catharina; Kellmann, Markus; Moehring, Thomas; Domon, Bruno

    2012-12-01

    There is an immediate need for improved methods to systematically and precisely quantify large sets of peptides in complex biological samples. To date protein quantification in biological samples has been routinely performed on triple quadrupole instruments operated in selected reaction monitoring mode (SRM), and two major challenges remain. Firstly, the number of peptides to be included in one survey experiment needs to be increased to routinely reach several hundreds, and secondly, the degree of selectivity should be improved so as to reliably discriminate the targeted analytes from background interferences. High resolution and accurate mass (HR/AM) analysis on the recently developed Q-Exactive mass spectrometer can potentially address these issues. This instrument presents a unique configuration: it is constituted of an orbitrap mass analyzer equipped with a quadrupole mass filter as the front-end for precursor ion mass selection. This configuration enables new quantitative methods based on HR/AM measurements, including targeted analysis in MS mode (single ion monitoring) and in MS/MS mode (parallel reaction monitoring). The ability of the quadrupole to select a restricted m/z range allows one to overcome the dynamic range limitations associated with trapping devices, and the MS/MS mode provides an additional stage of selectivity. When applied to targeted protein quantification in urine samples and benchmarked with the reference SRM technique, the quadrupole-orbitrap instrument exhibits similar or better performance in terms of selectivity, dynamic range, and sensitivity. This high performance is further enhanced by leveraging the multiplexing capability of the instrument to design novel acquisition methods and apply them to large targeted proteomic studies for the first time, as demonstrated on 770 tryptic yeast peptides analyzed in one 60-min experiment. The increased quality of quadrupole-orbitrap data has the potential to improve existing protein

  6. Determining gaseous composition of fluid inclusions with quadrupole mass spectrometer

    Institute of Scientific and Technical Information of China (English)

    ZHU; Heping

    2002-01-01

    [1]Joseph, R. G., Stephen, E. K., Factors affecting gas analysis of inclusion fluid by quadrupole mass spectrometry, Geo-chimica et Acta, 1995, 59(19): 3977-3986.[2]Masakatsu, S., Takayuki, S., Naoto, T., Analysis of fluid inclusion gases from geothermal systems, using a rapid-scanning quadrupole mass spectrometer, Eur. J. Mineral., 1992, 4: 895-906.[3]Van den Kerkhof, A. M., Isochoric phase diagrams in the systems CO2-CH4 and CO2-N2: Application to fluid inclusions, Geochimica et Cosmochimica Acta, 1990, 54: 621-629.[4]Colin, B., Michael, P. S., Mass spectrometric determination of gases in individual fluid inclusions in natural minerals, Anal. Chem., 1986, 58: 1330-1333.[5]David, I. N., Fredrick, J. S., Analysis of volatiles in fluid inclusions by mass spectrometry, Chemical Geology, 1987, 61: 1-10.[6]Yoichi, M., Ryo, K., Takayuki, S. et al., Gas composition of fluid inclusion from the Mori Geothermal Reservoir, South-western Hokkaido, Japan, Resource Geology, 1997, 47(5): 283-291.[7]Lu Huanzhang, Guo Dijiang, Progress and trends of researches on fluid inclusions, Geological Review, 2000, 46(4): 385-392.[8]Xia Xinyu, Wang Xianbin, Chen Jiangfeng, Geningjie, composition of fluid inclusions and CO2 carbon isotope of ultra-high pressure metamorphic rocks in Shuanghe area, Dabieshan Mountain, Science in China (in Chinese), Ser. D, 1999, 29(4): 314-320.

  7. Optimized Fast and Sensitive Acquisition Methods for Shotgun Proteomics on a Quadrupole Orbitrap Mass Spectrometer

    DEFF Research Database (Denmark)

    Kelstrup, Christian D; Young, Clifford; Lavallee, Richard;

    2012-01-01

    Advances in proteomics are continually driven by the introduction of new mass spectrometric instrumentation with improved performances. The recently introduced quadrupole Orbitrap (Q Exactive) tandem mass spectrometer allows fast acquisition of high-resolution higher-energy collisional dissociation...

  8. Newly developed apparatus for calibration of quadrupole mass spectrometer

    Science.gov (United States)

    Meng, Dong; Yongjun, Cheng; Detian, Li; Wenjun, Sun; Lan, Zhao; Meiru, Guo; Yongjun, Wang; Huzhong, Zhang; Yanwu, Li; Gang, Li

    2017-01-01

    In this paper, a new calibration apparatus has been developed for calibrating quadrupole mass spectrometer (QMS) from 10-8 Pa to 10-2 Pa for He, N2 and Ar. Based on the apparatus, two calibration methods are introduced to generate standard pressure P i ‧ (or P i ″) of lower than 10-2 Pa, which are named as ‘the SRG measurement method’ and ‘the CDG measurement method’. The SRG measurement method can generate a standard pressure range from 10-8 Pa to 10-5 Pa, and the CDG measurement method can generate a standard pressure range from 10-5 Pa to 10-2 Pa. A molecular flow condition is determined and a QMS is calibrated by the two methods using single gas and mixture gas. The gas flow through the small tube and orifice realizes molecular flow at an upstream pressure of less than 70 Pa. The sensitivities calibration results with the two methods agree well, and the difference is less than 3%. The sensitivity calibrated with single gas is different from that calibrated with mixture gas. Obtained results are roughly consistent with those of previous studies.

  9. Novel tandem quadrupole-acceleration-deceleration mass spectrometer for neutralization-reionization studies.

    Science.gov (United States)

    Turecek, F; Gu, M; Shaffer, S A

    1992-07-01

    A new tandem mass spectrometer of the quadrupole-acceleration lens-deceleration. lens-quadrupole (QADQ) configuration is described. The instrument is designed for neutralization-reionization studies and consists of a 2000-u quadrupole mass analyzer as MS-I, an acceleration electrostatic lens, a series of three differentially pumped collision cells, and an electrostatic deceleration lens, energy filter, and another 2000-u quadrupole mass analyzer as MS-II. The ion optical system achieves high total ion transmission for 5-9-keV ions. Unit mass resolution in neutralization-reionization mass spectra of aromatic compounds is demonstrated. Mass, kinetic energy, and linked scans at various levels of mass resolution and sensitivity are described.

  10. Direct trace analysis of metals and alloys in a quadrupole ion-trap mass spectrometer

    CERN Document Server

    Song, K S; Yang, M; Cha, H K; Lee, J M; Lee, G H

    1999-01-01

    An ion-trap mass spectrometer adopting a quadrupole ion-trap and laser ablation/ionization method was constructed. The developed system was tested for composition analysis of some metals (Cu, stainless), and alloys (hastalloy C, mumetal) by mass spectrometry. Samples were analyzed by using laser ablation from a sample probe tip followed by a mass analysis with the quadrupole ion-trap. The quadrupole ion-trap was modified to enable laser ablation by a XeCl excimer laser pulse that passed radially through the ring electrode. A mass scan of the produced ions was performed in the mass selective instability mode wherein trapped ions were successively detected by increasing the rf voltage through the ring electrode. Factors affecting the mass resolution, such as pressure of buffer gas and ablation laser power, are discussed.

  11. Targeted Proteomic Quantification on Quadrupole-Orbitrap Mass Spectrometer*

    OpenAIRE

    Gallien, Sebastien; Duriez, Elodie; Crone, Catharina; Kellmann, Markus; Moehring, Thomas; Domon, Bruno

    2012-01-01

    There is an immediate need for improved methods to systematically and precisely quantify large sets of peptides in complex biological samples. To date protein quantification in biological samples has been routinely performed on triple quadrupole instruments operated in selected reaction monitoring mode (SRM), and two major challenges remain. Firstly, the number of peptides to be included in one survey experiment needs to be increased to routinely reach several hundreds, and secondly, the degr...

  12. Quantitative proteomics using the high resolution accurate mass capabilities of the quadrupole-orbitrap mass spectrometer.

    Science.gov (United States)

    Gallien, Sebastien; Domon, Bruno

    2014-08-01

    High resolution/accurate mass hybrid mass spectrometers have considerably advanced shotgun proteomics and the recent introduction of fast sequencing capabilities has expanded its use for targeted approaches. More specifically, the quadrupole-orbitrap instrument has a unique configuration and its new features enable a wide range of experiments. An overview of the analytical capabilities of this instrument is presented, with a focus on its application to quantitative analyses. The high resolution, the trapping capability and the versatility of the instrument have allowed quantitative proteomic workflows to be redefined and new data acquisition schemes to be developed. The initial proteomic applications have shown an improvement of the analytical performance. However, as quantification relies on ion trapping, instead of ion beam, further refinement of the technique can be expected.

  13. HD gas analysis with Gas Chromatography and Quadrupole Mass Spectrometer

    CERN Document Server

    Ohta, T; Didelez, J -P; Fujiwara, M; Fukuda, K; Kohri, H; Kunimatsu, T; Morisaki, C; Ono, S; Rouille, G; Tanaka, M; Ueda, K; Uraki, M; Utsuro, M; Wang, S Y; Yosoi, M

    2011-01-01

    A gas analyzer system has been developed to analyze Hydrogen-Deuteride (HD) gas for producing frozen-spin polarized HD targets, which are used for hadron photoproduction experiments at SPring-8. Small amounts of ortho-H$_{2}$ and para-D$_{2}$ gas mixtures ($\\sim$0.01%) in the purified HD gas are a key to realize a frozen-spin polarized target. In order to obtain reliable concentrations of these gas mixtures in the HD gas, we produced a new gas analyzer system combining two independent measurements with the gas chromatography and the QMS. The para-H$_{2}$, ortho-H$_{2}$, HD, and D$_{2}$ are separated using the retention time of the gas chromatography and the mass/charge. It is found that the new gas analyzer system can measure small concentrations of $\\sim$0.01% for the otho-H$_2$ and D$_2$ with good S/N ratios.

  14. Mass separation of deuterium and helium with conventional quadrupole mass spectrometer by using varied ionization energy

    Science.gov (United States)

    Yu, Yaowei; Hu, Jiansheng; Wan, Zhao; Wu, Jinhua; Wang, Houyin; Cao, Bin

    2016-03-01

    Deuterium pressure in deuterium-helium mixture gas is successfully measured by a common quadrupole mass spectrometer (model: RGA200) with a resolution of ˜0.5 atomic mass unit (AMU), by using varied ionization energy together with new developed software and dedicated calibration for RGA200. The new software is developed by using MATLAB with the new functions: electron energy (EE) scanning, deuterium partial pressure measurement, and automatic data saving. RGA200 with new software is calibrated in pure deuterium and pure helium 1.0 × 10-6-5.0 × 10-2 Pa, and the relation between pressure and ion current of AMU4 under EE = 25 eV and EE = 70 eV is obtained. From the calibration result and RGA200 scanning with varied ionization energy in deuterium and helium mixture gas, both deuterium partial pressures (PD2) and helium partial pressure (PHe) could be obtained. The result shows that deuterium partial pressure could be measured if PD2 > 10-6 Pa (limited by ultimate pressure of calibration vessel), and helium pressure could be measured only if PHe/PD2 > 0.45, and the measurement error is evaluated as 15%. This method is successfully employed in EAST 2015 summer campaign to monitor deuterium outgassing/desorption during helium discharge cleaning.

  15. Correlation between y-type ions observed in ion trap and triple quadrupole mass spectrometers.

    Science.gov (United States)

    Sherwood, Carly A; Eastham, Ashley; Lee, Lik Wee; Risler, Jenni; Vitek, Olga; Martin, Daniel B

    2009-09-01

    Multiple reaction monitoring mass spectrometry (MRM-MS) is a technique for high-sensitivity targeted analysis. In proteomics, MRM-MS can be used to monitor and quantify a peptide based on the production of expected fragment peaks from the selected peptide precursor ion. The choice of which fragment ions to monitor in order to achieve maximum sensitivity in MRM-MS can potentially be guided by existing MS/MS spectra. However, because the majority of discovery experiments are performed on ion trap platforms, there is concern in the field regarding the generalizability of these spectra to MRM-MS on a triple quadrupole instrument. In light of this concern, many operators perform an optimization step to determine the most intense fragments for a target peptide on a triple quadrupole mass spectrometer. We have addressed this issue by targeting, on a triple quadrupole, the top six y-ion peaks from ion trap-derived consensus library spectra for 258 doubly charged peptides from three different sample sets and quantifying the observed elution curves. This analysis revealed a strong correlation between the y-ion peak rank order and relative intensity across platforms. This suggests that y-type ions obtained from ion trap-based library spectra are well-suited for generating MRM-MS assays for triple quadrupoles and that optimization is not required for each target peptide.

  16. Interfacing an ion mobility spectrometry based explosive trace detector to a triple quadrupole mass spectrometer.

    Science.gov (United States)

    Kozole, Joseph; Stairs, Jason R; Cho, Inho; Harper, Jason D; Lukow, Stefan R; Lareau, Richard T; DeBono, Reno; Kuja, Frank

    2011-11-15

    Hardware from a commercial-off-the-shelf (COTS) ion mobility spectrometry (IMS) based explosive trace detector (ETD) has been interfaced to an AB/SCIEX API 2000 triple quadrupole mass spectrometer. To interface the COTS IMS based ETD to the API 2000, the faraday plate of the IMS instrument and the curtain plate of the mass spectrometer were removed from their respective systems and replaced by a custom faraday plate, which was fabricated with a hole for passing the ion beam to the mass spectrometer, and a custom interface flange, which was designed to attach the IMS instrument onto the mass spectrometer. Additionally, the mass spectrometer was modified to increase the electric field strength and decrease the pressure in the differentially pumped interface, causing a decrease in the effect of collisional focusing and permitting a mobility spectrum to be measured using the mass spectrometer. The utility of the COTS-ETD/API 2000 configuration for the characterization of the gas phase ion chemistry of COTS-ETD equipment was established by obtaining mass and tandem mass spectra in the continuous ion flow and selected mobility monitoring operating modes and by obtaining mass-selected ion mobility spectra for the explosive standard 2,4,6 trinitrotoluene (TNT). This analysis confirmed that the product ion for TNT is [TNT - H](-), the predominant collision-induced dissociation pathway for [TNT- H](-) is the loss of NO and NO(2), and the reduced mobility value for [TNT - H](-) is 1.54 cm(2)V(-1) s(-1). Moreover, this analysis was attained for sample amounts of 1 ng and with a resolving power of 37. The objective of the research is to advance the operational effectiveness of COTS IMS based ETD equipment by developing a platform that can facilitate the understanding of the ion chemistry intrinsic to the equipment.

  17. Design and development of an interchangeable nanomicroelectrospray source for a quadrupole mass spectrometer

    Science.gov (United States)

    Smith, Douglas R.; Sagerman, Gary; Wood, Troy D.

    2003-10-01

    An interchangeable microelectrospray and nanoelectrospray ionization source has been designed and constructed for use on a triple-quadrupole mass spectrometer. This new source is specially designed to conduct nanoelectrospray experiments utilizing pulled borosilicate glass emitters, as well as various ionization modes utilizing silica capillaries. The source design facilitates the easy exchange between a microelectrospray source and nanoelectrospray source. The microionspray assembly can be quickly replaced by the nanoelectrospray adaptation in order to conduct nanoelectrospray experiments. Furthermore, this source design allows for the coupling of low flow separation techniques, like microliquid chromatography or capillary electrophoresis.

  18. A new method of alpha ray measurement using a Quadrupole Mass Spectrometer

    OpenAIRE

    Iwata, Y; Inoue, Y.; Minowa, M.

    2007-01-01

    We propose a new method of alpha($\\alpha$)-ray measurement that detects helium atoms with a Quadrupole Mass Spectrometer(QMS). A demonstration is undertaken with a plastic-covered $^{241}$Am $\\alpha$-emitting source to detect $\\alpha$-rays stopped in the capsule. We successfully detect helium atoms that diffuse out of the capsule by accumulating them for one to 20 hours in a closed chamber. The detected amount is found to be proportional to the accumulation time. Our method is applicable to p...

  19. Performance Characteristics of a New Hybrid Triple Quadrupole Time-of-Flight Tandem Mass Spectrometer

    Science.gov (United States)

    Andrews, Genna L.; Simons, Brigitte L.; Young, J. Bryce; Hawkridge, Adam M.; Muddiman, David C.

    2011-01-01

    The TripleTOF 5600 System, a hybrid triple quadrupole time-of-flight mass spectrometer, was evaluated to explore the key figures of merit in generating peptide and protein identifications which included spectral acquisition rates, data quality, proteome coverage, and biological depth. Employing a Saccharomyces cerevisiae tryptic digest, careful consideration of several performance features demonstrated that the speed of the TripleTOF contributed most to the resultant data. The TripleTOF system was operated with 8, 20, and 50 MS/MS events in an effort to compare to other MS technologies and to demonstrate the abilities of the instrument platform. PMID:21619048

  20. A new method of alpha ray measurement using a Quadrupole Mass Spectrometer

    OpenAIRE

    Iwata, Y.; Inoue, Y.; Minowa, M.

    2007-01-01

    We propose a new method of alpha($\\alpha$)-ray measurement that detects helium atoms with a Quadrupole Mass Spectrometer(QMS). A demonstration is undertaken with a plastic-covered $^{241}$Am $\\alpha$-emitting source to detect $\\alpha$-rays stopped in the capsule. We successfully detect helium atoms that diffuse out of the capsule by accumulating them for one to 20 hours in a closed chamber. The detected amount is found to be proportional to the accumulation time. Our method is applicable to p...

  1. Laser-induced acoustic desorption coupled with a linear quadrupole ion trap mass spectrometer.

    Science.gov (United States)

    Habicht, Steven C; Amundson, Lucas M; Duan, Penggao; Vinueza, Nelson R; Kenttämaa, Hilkka I

    2010-01-15

    In recent years, laser-induced acoustic desorption (LIAD) coupled with a Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer has been demonstrated to provide a valuable technique for the analysis of a wide variety of nonvolatile, thermally labile compounds, including analytes that could not previously be analyzed by mass spectrometry. Although FT-ICR instruments are very powerful, they are also large and expensive and, hence, mainly used as research instruments. In contrast, linear quadrupole ion trap (LQIT) mass spectrometers are common due to several qualities that make these instruments attractive for both academic and industrial settings, such as high sensitivity, large dynamic range, and experimental versatility. Further, the relatively small size of the instruments, comparatively low cost, and the lack of a magnetic field provide some distinct advantages over FT-ICR instruments. Hence, we have coupled the LIAD technique with a commercial LQIT, the Thermo Fischer Scientific LTQ mass spectrometer. The LQIT was modified for a LIAD probe by outfitting the removable back plate of the instrument with a 6 in. ConFlat flange (CFF) port, gate valve, and sample lock. Reagent ions were created using the LQIT's atmospheric pressure ionization source and trapped in the mass analyzer for up to 10 s to allow chemical ionization reactions with the neutral molecules desorbed via LIAD. These initial experiments focused on demonstrating the feasibility of performing LIAD in the LQIT. Hence, the results are compared to those obtained using an FT-ICR mass spectrometer. Despite the lower efficiency in the transfer of desorbed neutral molecules into the ion trap, and the smaller maximum number of available laser pulses, the intrinsically higher sensitivity of the LQIT resulted in a higher sensitivity relative to the FT-ICR.

  2. Implementation of Ion/Ion Reactions in a Quadrupole/Time-of-Flight Tandem Mass Spectrometer

    Science.gov (United States)

    Xia, Yu; Chrisman, Paul A.; Erickson, David E.; Liu, Jian; Liang, Xiaorong; Londry, Frank A.; Yang, Min J.; McLuckey, Scott A.

    2008-01-01

    A commercial quadrupole/time-of-flight (QqTOF) tandem mass spectrometer has been adapted for ion/ion reaction studies. To enable mutual storage of oppositely charged ions in a linear ion trap, the oscillating quadrupole field of the second quadrupole of the system (Q2) serves to store ions in the radial dimension while auxiliary RF is superposed on the end lenses of Q2 during the reaction period to create barriers in the axial dimension. A pulsed dual electrospray (ESI) source is directly coupled to the instrument interface for the purpose of proton transfer reactions. Singly and doubly charged protein ions as high in mass as 66 kDa are readily formed and observed after proton transfer reactions. For the modified instrument, the mass resolving power is about 8000 for a wide m/z range and the mass accuracy is ~20 ppm for external calibration and ~5 ppm for internal calibration after ion/ion reactions. Parallel ion parking is demonstrated with a six-component protein mixture, which shows the potential application of reducing spectral complexity and concentrating certain charge states. The current system has high flexibility with respect to defining MSn experiments involving collision-induced dissociation (CID) and ion/ion reactions. Protein precursor and CID product masses can be determined with good accuracy, providing an attractive platform for top-down proteomics. Electron transfer dissociation (ETD) ion/ion reactions are implemented by using a pulsed nano-ESI/atmospheric pressure chemical ionization (APCI) dual source for ionization. The reaction between protonated peptide ions and radical anions of 1,3-dinitrobenzene formed exclusively c- and z- type fragment ions. PMID:16771545

  3. Parallel reaction monitoring using quadrupole-Orbitrap mass spectrometer: Principle and applications.

    Science.gov (United States)

    Bourmaud, Adele; Gallien, Sebastien; Domon, Bruno

    2016-08-01

    Targeted mass spectrometry-based approaches are nowadays widely used for quantitative proteomics studies and more recently have been implemented on high resolution/accurate mass (HRAM) instruments resulting in a considerable performance improvement. More specifically, the parallel reaction monitoring technique (PRM) performed on quadrupole-Orbitrap mass spectrometers, leveraging the high resolution and trapping capabilities of the instrument, offers a clear advantage over the conventional selected reaction monitoring (SRM) measurements executed on triple quadrupole instruments. Analyses performed in HRAM mode allow for an improved discrimination between signals derived from analytes and those resulting from matrix interferences translating in the reliable quantification of low abundance components. The purpose of the study defines various implementation schemes of PRM, namely: (i) exploratory experiments assessing the detectability of very large sets of peptides (100-1000), (ii) wide-screen analyses using (crude) internal standards to obtain statistically meaningful (relative) quantitative analyses, and (iii) precise/accurate quantification of a limited number of analytes using calibrated internal standards. Each of the three implementation schemes requires specific acquisition methods with defined parameters to appropriately control the acquisition during the actual peptide elution. This tutorial describes the different PRM approaches and discusses their benefits and limitations in terms of quantification performance and confidence in analyte identification.

  4. Insertion of an electron beam ionizer in a quadrupole spectrometer for secondary neutral mass analysis

    CERN Document Server

    Ameziane, O; Serrano, J; Guzman, B; Aguilar, M A

    2003-01-01

    An insertable electron beam ionizer into a quadrupole-based secondary ion mass spectrometer instrument has been designed and installed to analyze sputtered neutrals. The optimum design conditions of the ionizer have been obtained by modeling various configurations of the system using a simulation program developed by us. The program has allowed us to compute the potentials and ion trajectories inside the system to test the performance of the ion optics design. We have investigated the advantages of using a large ionization volume with low electron current to minimize the space charge effect in the ionizer, as this is the major problem in this type of instrument. In addition, we have used the simulations to obtain' all electrodes voltages which provide an efficient suppression of residual gas and secondary ions. A good useful yield was obtained, even with low electron densities, thanks to the high geometrical acceptance of the ionizer and its large active volume. This configuration implies less thermal radiati...

  5. Ion-neutral transport through quadrupole interfaces of mass-spectrometer systems

    Energy Technology Data Exchange (ETDEWEB)

    Jugroot, M.; Groth, C.P.T. [Univ. of Toronto, Inst. for Aerospace Studies, Toronto, Ontario (Canada)]. E-mail: jugroot@utias.utoronto.ca; groth@utias.utoronto.ca; Thomson, B.A.; Baranov, V.; Collings, B.A.; French, J.B. [MDS SCIEX, Concord, Ontario (Canada)

    2004-07-01

    The transport of free ions through highly under-expanded jet flows of neutral gases and in the presence of applied electric fields is investigated by continuum-based numerical simulations. In particular, numerical results are described which are relevant to ion flows occurring in quadrupole interfaces of mass spectrometer systems. A five-moment mathematical model and parallel multi-block numerical solution procedure is developed for predicting the ion transport. The model incorporates the effects of ion-neutral collision processes and is used in conjunction with a Navier-Stokes model and flow solver for the neutral gas to examine the key influences controlling the ion motion. The effects of the neutral gas flow, electric fields (both dc and rf), and flow field geometry on ion mobility are carefully assessed. The capability of controlling the charged particle motions through a combination of directed neutral flow and applied electric field is demonstrated for these high-speed, hypersonic, jet flows. (author)

  6. Proteomic analysis of Vibrio metschnikovii under cold stress using a quadrupole Orbitrap mass spectrometer.

    Science.gov (United States)

    Jia, Juntao; Chen, Ying; Jiang, Yinghui; Li, Zhengyi; Zhao, Liqing; Zhang, Jian; Tang, Jing; Feng, Liping; Liang, Chengzhu; Xu, Biao; Gu, Peiming; Ye, Xiwen

    2015-10-01

    Vibrio metschnikovii is a food-borne pathogen found in seafood worldwide. We studied the global proteome responses of V. metschnikovii under cold stress by nano-flow ultra-high-performance liquid chromatography coupled to a quadrupole Orbitrap mass spectrometer. A total of 2066 proteins were identified, among which 288 were significantly upregulated and 572 were downregulated. Functional categorization of these proteins revealed distinct differences between cold-stressed and control cells. Quantitative reverse transcription polymerase chain reaction analysis was also performed to determine the mRNA expression levels of seventeen cold stress-related genes. The results of this study should improve our understanding of the metabolic activities of cold-adapted bacteria and will facilitate a better systems-based understanding of V. metschnikovii.

  7. A study of resonance electron capture ionization on a quadrupole tandem mass spectrometer.

    Science.gov (United States)

    Wei, J; Liu, S; Fedoreyev, S A; Voinov, V G

    2000-01-01

    Procedures that allow the realization of resonance electron capture (REC) mode on a commercial triple-quadrupole mass spectrometer, after some simple modifications, are described. REC mass spectrometry (MS) and tandem mass spectrometry (MS/MS) experiments were performed and spectra for some compounds were recorded. In particular, the charge-remote fragmentation (CRF) spectra of [M - H](-) ions of docosanoic and docosenoic acids under low-energy collisionally activated dissociation (CAD) conditions were obtained, and showed that there were no significant differences for [M - H](-) ions produced at different resonances (i.e. for [M - H](-) ions with different structures). This observation was explained on the basis of results obtained from deuterium-labeled fatty acids, which showed that different CRF ions (but with the same m/z value in the absence of labels) could be produced by different mechanisms, and all of them were obviously realized under CAD conditions that made spectra practically indistinguishable. The other example, which compared the REC-MS/MS spectrum of [M - H](-) ions and EI-MS/MS spectrum of M(+.) ions of daidzein, demonstrated the potential of the REC-MS/MS technique for more complex structure elucidation.

  8. Microfluidic cell culture and metabolism detection with electrospray ionization quadrupole time-of-flight mass spectrometer.

    Science.gov (United States)

    Gao, Dan; Wei, Huibin; Guo, Guang-Sheng; Lin, Jin-Ming

    2010-07-01

    A novel method for the characterization of drug metabolites was developed by integrating chip-based solid-phase extraction (SPE) with an online electrospray ionization quadrupole time-of-fight mass spectrometer (ESI-Q-TOF-MS). The integrated microfluidic device was composed of circular chambers for cell culture and straight microchannels with shrink ends to pack the solid-phase material for sample cleanup and concentration prior to mass analysis. By connecting the two separated microchannels with polyethylene tubes, drug metabolism studies related to functional units, including cell culture, metabolism generation, sample pretreatment, and detection, were all integrated into the microfluidic device. To verify the feasibility of a drug metabolism study on the microfluidic device, the metabolism of vitamin E in human lung epithelial A549 cells was studied. The metabolites were successfully detected by online ESI-Q-TOF-MS with high sensitivity and short analysis time (8 min). By integrating several parallel channels, the desalting and concentration process could be simultaneously achieved. The total sample pretreatment time only needed about 15 min, and solvent consumption could be reduced to less than 100 microL. All this demonstrated that the developed microfluidic device could be a potential useful tool for cellular drug metabolism research.

  9. Initial SAM Calibration Gas Experiments on Mars: Quadrupole Mass Spectrometer Results and Implications

    Science.gov (United States)

    Franz, Heather B.; Trainer, Melissa G.; Malespin, Charles A.; Mahaffy, Paul R.; Atreya, Sushil K.; Becker, Richard H,; Benna, Mehdi; Conrad, Pamela G.; Eigenbrode, Jennifer L.; Freissinet, Caroline; hide

    2017-01-01

    The Sample Analysis at Mars (SAM) instrument suite of the Mars Science Laboratory (MSL) Curiosity rover is equipped to analyze both martian atmospheric gases and volatiles released by pyrolysis of solid surface materials, with target measurements including chemical and isotopic composition (Mahaffy et al., 2012). To facilitate assessment of instrument performance and validation of results obtained on Mars, SAM houses a calibration cell containing CO2, Ar, N2, Xe, and several fluorinated hydrocarbon compounds (Franz et al., 2014; Mahaffy et al., 2012). This report describes the first two experiments utilizing this calibration cell on Mars and gives results from analysis of data acquired with the SAM Quadrupole Mass Spectrometer (QMS). These data support the accuracy of isotope ratios obtained with the QMS (Conrad et al., 2016; Mahaffy et al., 2013) and provide ground-truth for reassessment of analytical constants required for atmospheric measurements, which were reported in previous contributions (Franz et al., 2015, 2014). The most significant implication of the QMS data involves reinterpretation of pre-launch contamination previously believed to affect only CO abundance measurements (Franz et al., 2015) to affect N2 abundances, as well. The corresponding adjustment to the N2 calibration constant presented here brings the atmospheric volume mixing ratios for Ar and N2 retrieved by SAM into closer agreement with those reported by the Viking mission (Owen et al., 1977; Oyama and Berdahl, 1977).

  10. Initial SAM calibration gas experiments on Mars: Quadrupole mass spectrometer results and implications

    Science.gov (United States)

    Franz, Heather B.; Trainer, Melissa G.; Malespin, Charles A.; Mahaffy, Paul R.; Atreya, Sushil K.; Becker, Richard H.; Benna, Mehdi; Conrad, Pamela G.; Eigenbrode, Jennifer L.; Freissinet, Caroline; Manning, Heidi L. K.; Prats, Benito D.; Raaen, Eric; Wong, Michael H.

    2017-04-01

    The Sample Analysis at Mars (SAM) instrument suite of the Mars Science Laboratory (MSL) Curiosity rover is equipped to analyze both martian atmospheric gases and volatiles released by pyrolysis of solid surface materials, with target measurements including chemical and isotopic composition (Mahaffy et al., 2012). To facilitate assessment of instrument performance and validation of results obtained on Mars, SAM houses a calibration cell containing CO2, Ar, N2, Xe, and several fluorinated hydrocarbon compounds (Franz et al., 2014; Mahaffy et al., 2012). This report describes the first two experiments utilizing this calibration cell on Mars and gives results from analysis of data acquired with the SAM Quadrupole Mass Spectrometer (QMS). These data support the accuracy of isotope ratios obtained with the QMS (Conrad et al., 2016; Mahaffy et al., 2013) and provide ground-truth for reassessment of analytical constants required for atmospheric measurements, which were reported in previous contributions (Franz et al., 2015, 2014). The most significant implication of the QMS data involves reinterpretation of pre-launch contamination previously believed to affect only CO abundance measurements (Franz et al., 2015) to affect N2 abundances, as well. The corresponding adjustment to the N2 calibration constant presented here brings the atmospheric volume mixing ratios for Ar and N2 retrieved by SAM into closer agreement with those reported by the Viking mission (Owen et al., 1977; Oyama and Berdahl, 1977).

  11. High-throughput mass-directed parallel purification incorporating a multiplexed single quadrupole mass spectrometer.

    Science.gov (United States)

    Xu, Rongda; Wang, Tao; Isbell, John; Cai, Zhe; Sykes, Christopher; Brailsford, Andrew; Kassel, Daniel B

    2002-07-01

    We report on the development of a parallel HPLC/MS purification system incorporating an indexed (i.e., multiplexed) ion source. In the method described, each of the flow streams from a parallel array of HPLC columns is directed toward the multiplexed (MUX) ion source and sampled in a time-dependent, parallel manner. A visual basic application has been developed and monitors in real-time the extracted ion current from each sprayer channel. Mass-directed fraction collection is initiated into a parallel array of fraction collectors specific for each of the spray channels. In the first embodiment of this technique, we report on a four-column semipreparative parallel LC/MS system incorporating MUX detection. In this parallel LC/MS application (in which sample loads between 1 and 10 mg on-column are typically made), no cross talk was observed. Ion signals from each of the channels were found reproducible over 192 injections, with interchannel signal variations between 11 and 17%. The visual basic fraction collection application permits preset individual start collection and end collection thresholds for each channel, thereby compensating for the slight variation in signal between sprayers. By incorporating postfraction collector UV detection, we have been able to optimize the valve-triggering delay time with precut transfer tubing between the mass spectrometer and fraction collectors and achieve recoveries greater than 80%. Examples of the MUX-guided, mass-directed fraction purification of both standards and real library reaction mixtures are presented within.

  12. Investigation of Ion Transmission Effects on Intact Protein Quantification in a Triple Quadrupole Mass Spectrometer

    Science.gov (United States)

    Wang, Evelyn H.; Appulage, Dananjaya Kalu; McAllister, Erin A.; Schug, Kevin A.

    2017-09-01

    Recently, direct intact protein quantitation using triple quadrupole mass spectrometry (QqQ-MS) and multiple reaction monitoring (MRM) was demonstrated (J. Am. Soc. Mass Spectrom. 27, 886-896 (2016)). Even though QqQ-MS is known to provide extraordinary detection sensitivity for quantitative analysis, we found that intact proteins exhibited a less than 5% ion transmission from the first quadrupole to the third quadrupole mass analyzer in the presence of zero collision energy (ZCE). With the goal to enhance intact protein quantitation sensitivity, ion scattering effects, proton transfer effects, and mass filter resolution widths were examined for their contributions to the lost signal. Protein standards myoglobin and ubiquitin along with small molecules reserpine and vancomycin were analyzed together with various collision induced dissociation (CID) gases (N2, He, and Ar) at different gas pressures. Mass resolution settings played a significant role in reducing ion transmission signal. By narrowing the mass resolution window by 0.35 m/z on each side, roughly 75%-90% of the ion signal was lost. The multiply charged proteins experienced additional proton transfer effects, corresponding to 10-fold signal reduction. A study of increased sensitivity of the method was also conducted with various MRM summation techniques. Although the degree of enhancement was analyte-dependent, an up to 17-fold increase in sensitivity was observed for ubiquitin using a summation of multiple MRM transitions. Biological matrix, human urine, and equine plasma were spiked with proteins to demonstrate the specificity of the method. This study provides additional insight into optimizing the use and sensitivity of QqQ-MS for intact protein quantification. [Figure not available: see fulltext.

  13. Infrared ion spectroscopy in a modified quadrupole ion trap mass spectrometer at the FELIX free electron laser laboratory

    Science.gov (United States)

    Martens, Jonathan; Berden, Giel; Gebhardt, Christoph R.; Oomens, Jos

    2016-10-01

    We report on modifications made to a Paul-type quadrupole ion trap mass spectrometer and discuss its application in infrared ion spectroscopy experiments. Main modifications involve optical access to the trapped ions and hardware and software coupling to a variety of infrared laser sources at the FELIX infrared free electron laser laboratory. In comparison to previously described infrared ion spectroscopy experiments at the FELIX laboratory, we find significant improvements in efficiency and sensitivity. Effects of the trapping conditions of the ions on the IR multiple photon dissociation spectra are explored. Enhanced photo-dissociation is found at lower pressures in the ion trap. Spectra obtained under reduced pressure conditions are found to more closely mimic those obtained in the high-vacuum conditions of an Fourier transform ion cyclotron resonance mass spectrometer. A gas-mixing system is described enabling the controlled addition of a secondary gas into helium buffer gas flowing into the trap and allows for ion/molecule reactions in the trap. The electron transfer dissociation (ETD) option of the mass spectrometer allows for IR structure characterization of ETD-generated peptide dissociation products.

  14. Multiple Reaction Monitoring for Direct Quantitation of Intact Proteins Using a Triple Quadrupole Mass Spectrometer.

    Science.gov (United States)

    Wang, Evelyn H; Combe, Peter C; Schug, Kevin A

    2016-05-01

    Methods that can efficiently and effectively quantify proteins are needed to support increasing demand in many bioanalytical fields. Triple quadrupole mass spectrometry (QQQ-MS) is sensitive and specific, and it is routinely used to quantify small molecules. However, low resolution fragmentation-dependent MS detection can pose inherent difficulties for intact proteins. In this research, we investigated variables that affect protein and fragment ion signals to enable protein quantitation using QQQ-MS. Collision induced dissociation gas pressure and collision energy were found to be the most crucial variables for optimization. Multiple reaction monitoring (MRM) transitions for seven standard proteins, including lysozyme, ubiquitin, cytochrome c from both equine and bovine, lactalbumin, myoglobin, and prostate-specific antigen (PSA) were determined. Assuming the eventual goal of applying such methodology is to analyze protein in biological fluids, a liquid chromatography method was developed. Calibration curves of six standard proteins (excluding PSA) were obtained to show the feasibility of intact protein quantification using QQQ-MS. Linearity (2-3 orders), limits of detection (0.5-50 μg/mL), accuracy (protein. Sensitivities for different proteins varied considerably. Biological fluids, including human urine, equine plasma, and bovine plasma were used to demonstrate the specificity of the approach. The purpose of this model study was to identify, study, and demonstrate the advantages and challenges for QQQ-MS-based intact protein quantitation, a largely underutilized approach to date.

  15. Multiple Reaction Monitoring for Direct Quantitation of Intact Proteins Using a Triple Quadrupole Mass Spectrometer

    Science.gov (United States)

    Wang, Evelyn H.; Combe, Peter C.; Schug, Kevin A.

    2016-05-01

    Methods that can efficiently and effectively quantify proteins are needed to support increasing demand in many bioanalytical fields. Triple quadrupole mass spectrometry (QQQ-MS) is sensitive and specific, and it is routinely used to quantify small molecules. However, low resolution fragmentation-dependent MS detection can pose inherent difficulties for intact proteins. In this research, we investigated variables that affect protein and fragment ion signals to enable protein quantitation using QQQ-MS. Collision induced dissociation gas pressure and collision energy were found to be the most crucial variables for optimization. Multiple reaction monitoring (MRM) transitions for seven standard proteins, including lysozyme, ubiquitin, cytochrome c from both equine and bovine, lactalbumin, myoglobin, and prostate-specific antigen (PSA) were determined. Assuming the eventual goal of applying such methodology is to analyze protein in biological fluids, a liquid chromatography method was developed. Calibration curves of six standard proteins (excluding PSA) were obtained to show the feasibility of intact protein quantification using QQQ-MS. Linearity (2-3 orders), limits of detection (0.5-50 μg/mL), accuracy (protein. Sensitivities for different proteins varied considerably. Biological fluids, including human urine, equine plasma, and bovine plasma were used to demonstrate the specificity of the approach. The purpose of this model study was to identify, study, and demonstrate the advantages and challenges for QQQ-MS-based intact protein quantitation, a largely underutilized approach to date.

  16. Biological tissue imaging with a hybrid cluster SIMS quadrupole time-of-flight mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Carado, A. [Pennsylvania State University, 104 Chemistry Building, University Park, PA (United States)], E-mail: ajc161@psu.edu; Kozole, J.; Passarelli, M.; Winograd, N. [Pennsylvania State University, 104 Chemistry Building, University Park, PA (United States); Loboda, A. [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ontario, CA (United States); Bunch, J. [Centre for Analytical Sciences, University of Sheffield, Sheffield S3 7HF (United Kingdom); Wingate, J. [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ontario, CA (United States); Hankin, J.; Murphy, R. [University of Colorado at Denver and Health Science Center, 12801 East 17th Avenue, Aurora, CO (United States)

    2008-12-15

    A 20 keV C{sub 60}{sup +} ion source was mounted onto a commercial MALDI/electrospray orthogonal ToF mass spectrometer. Cross-sectional mouse brain and lung slices between 5 and 10 {mu}m prepared by cryostat sectioning were successfully imaged using a DC C{sub 60}{sup +} primary ion beam at a spot size of 100 {mu}m. Analysis was performed at room temperature following vacuum drying. An abundance of ions were mapped in all samples, many whose identity can only be found using the MS/MS functionality. We have successfully identified and imaged localizations of diacylglycerol (DAG) ions - 1-palmitoyl-2-oleoyl-glycerol (m/z{sup +} 577.5) and 1,2-dioleoyl-glycerol (m/z{sup +} 603.5) - in lung tissue. The mouse brain slice revealed strong, distinct localizations of many ions revealing the potential for this technique for biological imaging. Ions throughout the mass range of m/z{sup +} 50-800 were collected in sufficient quantities to permit unambiguous chemical mapping. Mass resolutions of 12,000 or greater were routinely obtained allowing for more accurate ion mapping than typically seen with ToF-SIMS image analysis.

  17. LIGA Technology and Its Application in Miniature Quadrupole Mass Spectrometer Array%LIGA技术及其在四级质谱计阵列微型化中的应用

    Institute of Scientific and Technical Information of China (English)

    丁军平; 周抗寒; 黄刚; 凌波; 刘学博

    2004-01-01

    The quadrupole mass spectrometer array (QMSA) is the most important embranchment in the miniaturization of the quadrupole mass spectrometer (QMS). Making miniature mass filter is one of the key technology in the manufacture of QMSA. In this paper, the method of LIGA technology and its application in making mass spectrometer are introduced. This resolve radically the question how to making a miniature QMS in volume, weight, power and cost.

  18. Characterization and performance of MALDI on a triple quadrupole mass spectrometer for analysis and quantification of small molecules.

    Science.gov (United States)

    Gobey, Jason; Cole, Mark; Janiszewski, John; Covey, Thomas; Chau, Tung; Kovarik, Peter; Corr, Jay

    2005-09-01

    The usefulness of MALDI for small-molecule work has been limited by matrix chemical interference in the mass range of interest, tedious sample preparation, and various crystallization and sample deposition issues. We report instrument characterization and small-molecule quantification performance data from a high repetition rate laser MALDI ion source coupled to a triple quadrupole mass spectrometer. The high repetition rate laser improves sensitivity and precision and allows a proportional increase in sample throughput. Tandem mass spectrometry is used to discriminate the signal from the high chemical background caused by the MALDI matrix. Successful quantification requires use of an internal standard and a means of sample cleanup for typical in vitro sample compositions. This instrument combination and analysis technique is relatively insensitive to sample crystal quality and spot homogeneity. Quantitative performance results are characterized for 53 small-molecule pharmaceutical compounds and compared to those obtained by ESI-MS/MS. Further comparison between MALDI and ESI is examined, and the potential for high-throughput MALDI-MS/MS quantification is demonstrated.

  19. Positive ion chemistry in the exhaust plumes of an air craft jet engine and a burner: investigations with a quadrupole ion trap mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Kiendler, A.; Aberle, S.; Arnold, F. [Max Planck Institute for Nuclear Physics, Heidelberg (Germany). Atmospheric Physics Div.

    2000-07-01

    Using a quadrupole ion trap mass spectrometer detailed composition analyses were made of positive ions in the exhaust of an aircraft jet engine and of a jet fuel burner. For both scenarios complex organic ions with large mass numbers were most abundant. By employing the MS{sup 2}-mode of the quadrupole ion trap mass spectrometer, mass selected trapped ions were intendently broken up and characteristic fragment ions were observed. The latter indicate that the parent ions contain hydrogen, carbon and oxygen which is indicative of oxygenated hydrocarbons. This contrasts recent composition measurements of negative ions in aircraft jet engine exhaust made by our group which revealed that negative ions contain the inorganic acid H{sub 2}SO{sub 4}. Our present measurements support the view that positive ions in aircraft jet engine exhaust contain preferably organic molecules. (author)

  20. Quantitation of isobaric phosphatidylcholine species in human plasma using a hybrid quadrupole linear ion-trap mass spectrometer.

    Science.gov (United States)

    Zacek, Petr; Bukowski, Michael; Rosenberger, Thad A; Picklo, Matthew

    2016-12-01

    Phosphatidylcholine (PC) species in human plasma are used as biomarkers of disease. PC biomarkers are often limited by the inability to separate isobaric PCs. In this work, we developed a targeted shotgun approach for analysis of isobaric and isomeric PCs. This approach is comprised of two MS methods: a precursor ion scanning (PIS) of mass m/z 184 in positive mode (PIS m/z +184) and MS(3) fragmentation in negative mode, both performed on the same instrument, a hybrid triple quadrupole ion-trap mass spectrometer. The MS(3) experiment identified the FA composition and the relative abundance of isobaric and sn-1, sn-2 positional isomeric PC species, which were subsequently combined with absolute quantitative data obtained by PIS m/z +184 scan. This approach was applied to the analysis of a National Institute of Standards and Technology human blood plasma standard reference material (SRM 1950). We quantified more than 70 PCs and confirmed that a majority are present in isobaric and isomeric mixtures. The FA content determined by this method was comparable to that obtained using GC with flame ionization detection, supporting the quantitative nature of this MS method. This methodology will provide more in-depth biomarker information for clinical and mechanistic studies.

  1. Comprehensive lipidome analysis by shotgun lipidomics on a hybrid quadrupole-orbitrap-linear ion trap mass spectrometer.

    Science.gov (United States)

    Almeida, Reinaldo; Pauling, Josch Konstantin; Sokol, Elena; Hannibal-Bach, Hans Kristian; Ejsing, Christer S

    2015-01-01

    Here we report on the application of a novel shotgun lipidomics platform featuring an Orbitrap Fusion mass spectrometer equipped with an automated nanoelectrospray ion source. To assess the performance of the platform for in-depth lipidome analysis, we evaluated various instrument parameters, including its high resolution power unsurpassed by any other contemporary Orbitrap instrumentation, its dynamic quantification range and its efficacy for in-depth structural characterization of molecular lipid species by quadrupole-based higher-energy collisional dissociation (HCD), and ion trap-based resonant-excitation collision-induced dissociation (CID). This evaluation demonstrated that FTMS analysis with a resolution setting of 450,000 allows distinguishing isotopes from different lipid species and features a linear dynamic quantification range of at least four orders of magnitude. Evaluation of fragmentation analysis demonstrated that combined use of HCD and CID yields complementary fragment ions of molecular lipid species. To support global lipidome analysis, we designed a method, termed MS(ALL), featuring high resolution FTMS analysis for lipid quantification, and FTMS(2) analysis using both HCD and CID and ITMS(3) analysis utilizing dual CID for in-depth structural characterization of molecular glycerophospholipid species. The performance of the MS(ALL) method was benchmarked in a comparative analysis of mouse cerebellum and hippocampus. This analysis demonstrated extensive lipidome quantification covering 311 lipid species encompassing 20 lipid classes, and identification of 202 distinct molecular glycerophospholipid species when applying a novel high confidence filtering strategy. The work presented here validates the performance of the Orbitrap Fusion mass spectrometer for in-depth lipidome analysis.

  2. Determinations of airborne synthetic musks by polyurethane foam coupled with triple quadrupole gas chromatography tandem mass spectrometer.

    Science.gov (United States)

    Wang, I-Ting Ivy; Cheng, Shu-Fang; Tsai, Shih-Wei

    2014-02-21

    Synthetic musk is widely used in various scented consumer products. However, the exposure via inhalation is often ignored due to pleasant smells. In addition, the information regarding the distribution of synthetic musk in air is limited. Hence, this research is aimed to develop a highly sensitive and widely applicable method for the determination of airborne synthetic musk. In this study, polyurethane foam (PUF) and filter were employed for active air sampling. Microwave assisted extraction (MAE) and nitrogen evaporator were performed for sample preparation. A gas chromatography coupled with triple quadrupole tandem mass spectrometer (GC/MS-MS) with specific multiple reaction monitoring (MRM) transition pairs was applied for sample analysis. Compared with using selected ion monitoring (SIM) mode traditionally, the sensitivities were improved in this study about an order at least. In terms of air concentration, as low as 0.48ngm(-3) can be determined when sampling at 3.5Lmin(-1) for 8h. The method established was further applied to the analysis of synthetic musk compounds in air samples collected in a cosmetics plant. The results showed that the airborne concentrations of gaseous polycyclic musk, gaseous nitro-musk, and particle-phase polycyclic musk were 6.4×10(2), 4.0×10(1) and 3.1×10(2)ngm(-3), respectively. Meanwhile, Cashmeran, Celstolide, Galaxolide, and Tonalide were found as the dominant musk compounds in the factory investigated.

  3. Carbon and Sulfur Isotopic Composition of Yellowknife Bay Sediments: Measurements by the Sample Analysis at Mars (SAM) Quadrupole Mass Spectrometer

    Science.gov (United States)

    Franz, H. B.; Mahaffy, P. R.; Stern, J. C.; Eigenbrode, J. L.; Steele, A.; Ming, D. W.; McAdam, A. C.; Freissinet, C.; Glavin, D. P.; Archer, P. D.; Brunner, A. E.; Grotzinger,J. P.; Jones, J. H.; Leshin, L. A.; Miller, K.; Morris, R. V.; Navarro-Gonzalez, R.; Niles, P. B.; Owen, T. C.; Summons, R. E.; Sutter, B.; Webster, C. R.

    2014-01-01

    Since landing at Gale Crater in Au-gust 2012, the Sample Analysis at Mars (SAM) instru-ment suite on the Mars Science Laboratory (MSL) “Curiosity” rover has analyzed solid samples from the martian regolith in three locations, beginning with a scoop of aeolian deposits from the Rocknest (RN) sand shadow. Curiosity subsequently traveled to Yellowknife Bay, where SAM analyzed samples from two separate holes drilled into the Sheepbed Mudstone, designated John Klein (JK) and Cumberland (CB). Evolved gas analysis (EGA) of all samples revealed the presence of H2O as well as O-, C- and S-bearing phas-es, in most cases at abundances below the detection limit of the CheMin instrument. In the absence of definitive mineralogical identification by CheMin, SAM EGA data can help provide clues to the mineralogy of volatile-bearing phases through examination of tem-peratures at which gases are evolved from solid sam-ples. In addition, the isotopic composition of these gas-es may be used to identify possible formation scenarios and relationships between phases. Here we report C and S isotope ratios for CO2 and SO2 evolved from the JK and CB mudstone samples as measured with SAM’s quadrupole mass spectrometer (QMS) and draw com-parisons to RN.

  4. Correlation between y-Type Ions Observed in Ion Trap and Triple Quadrupole Mass Spectrometers

    OpenAIRE

    Sherwood, Carly A.; Eastham, Ashley; Lee, Lik Wee; Risler, Jenni; Vitek, Olga; Martin, Daniel B.

    2009-01-01

    Multiple reaction monitoring mass spectrometry (MRM-MS) is a technique for high-sensitivity targeted analysis. In proteomics, MRM-MS can be used to monitor and quantify a peptide based on the production of expected fragment peaks from the selected peptide precursor ion. The choice of which fragment ions to monitor in order to achieve maximum sensitivity in MRM-MS can potentially be guided by existing MS/MS spectra. However, because the majority of discovery experiments are performed on ion tr...

  5. Cluster SIMS with a hybrid quadrupole time-of-flight mass spectrometer

    Science.gov (United States)

    Carado, A.; Kozole, J.; Passarelli, M.; Winograd, N.; Loboda, A.; Wingate, J.

    2008-12-01

    The new physics associated with cluster SIMS, i.e. reduced chemical damage enabling 3D dynamic imaging, and increased ion yields from organics samples, suggests that cluster sources may be suitable for use on commercial MALDI/electrospray (ESI) instruments. In efforts to investigate this approach to secondary ion analysis, a 20 keV C 60+ primary ion source by Ionoptika Ltd. was fitted to a commercial LC/MS/MS instrument; the QSTAR ® XL system by Applied Biosystems/MDS Sciex. This instrument is capable of MS/MS, ion trapping, chemical imaging, and utilizes an orthogonal ToF, enabling use of a DC primary ion beam for imaging and data collection. The system employs high nitrogen pressure, typically several millitorr, in the sample region, as opposed to large extraction voltages, to facilitate the transmission of the secondary ions to the ToF region. In these initial experiments, it was demonstrated that ion signal generated by C 60+ bombardment can be enhanced by trapping in the collision cell and that secondary ions can fragment via collision induced dissociation (CID) to yield MS/MS information. In ToF-MS mode, efficiencies are comparable with pulsed primary beam ToF-SIMS instruments. Mass resolution of over 12,000 is routinely observed with mass accuracy in the 2 ppm range, which has important implications in accurate ion mapping in imaging mode.

  6. Cluster SIMS with a hybrid quadrupole time-of-flight mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Carado, A. [Pennsylvania State University, 104 Chemistry Building, University Park, PA 16802 (United States)], E-mail: ajc161@psu.edu; Kozole, J.; Passarelli, M.; Winograd, N. [Pennsylvania State University, 104 Chemistry Building, University Park, PA 16802 (United States); Loboda, A.; Wingate, J. [Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ontario, CA (United States)

    2008-12-15

    The new physics associated with cluster SIMS, i.e. reduced chemical damage enabling 3D dynamic imaging, and increased ion yields from organics samples, suggests that cluster sources may be suitable for use on commercial MALDI/electrospray (ESI) instruments. In efforts to investigate this approach to secondary ion analysis, a 20 keV C{sub 60}{sup +} primary ion source by Ionoptika Ltd. was fitted to a commercial LC/MS/MS instrument; the QSTAR XL system by Applied Biosystems/MDS Sciex. This instrument is capable of MS/MS, ion trapping, chemical imaging, and utilizes an orthogonal ToF, enabling use of a DC primary ion beam for imaging and data collection. The system employs high nitrogen pressure, typically several millitorr, in the sample region, as opposed to large extraction voltages, to facilitate the transmission of the secondary ions to the ToF region. In these initial experiments, it was demonstrated that ion signal generated by C{sub 60}{sup +} bombardment can be enhanced by trapping in the collision cell and that secondary ions can fragment via collision induced dissociation (CID) to yield MS/MS information. In ToF-MS mode, efficiencies are comparable with pulsed primary beam ToF-SIMS instruments. Mass resolution of over 12,000 is routinely observed with mass accuracy in the 2 ppm range, which has important implications in accurate ion mapping in imaging mode.

  7. MASS SPECTROMETER

    Science.gov (United States)

    White, F.A.

    1960-08-23

    A mass spectrometer is designed with a first adjustable magnetic field for resolving an ion beam into beams of selected masses, a second adjustable magnetic field for further resolving the ion beam from the first field into beams of selected masses, a thin foil disposed in the path of the beam between the first and second magnets to dissociate molecular ions incident thereon, an electrostatic field for further resolving the ion beam from the second field into beams of selected masses, and a detector disposed adjacent to the electrostatic field to receive the ion beam.

  8. Rapid 'de novo' peptide sequencing by a combination of nanoelectrospray, isotopic labeling and a quadrupole/time-of-flight mass spectrometer.

    Science.gov (United States)

    Shevchenko, A; Chernushevich, I; Ens, W; Standing, K G; Thomson, B; Wilm, M; Mann, M

    1997-01-01

    Protein microanalysis usually involves the sequencing of gel-separated proteins available in very small amounts. While mass spectrometry has become the method of choice for identifying proteins in databases, in almost all laboratories 'de novo' protein sequencing is still performed by Edman degradation. Here we show that a combination of the nanoelectrospray ion source, isotopic end labeling of peptides and a quadrupole/ time-of-flight instrument allows facile read-out of the sequences of tryptic peptides. Isotopic labeling was performed by enzymatic digestion of proteins in 1:1 16O/18O water, eliminating the need for peptide derivatization. A quadrupole/time-of-flight mass spectrometer was constructed from a triple quadrupole and an electrospray time-of-flight instrument. Tandem mass spectra of peptides were obtained with better than 50 ppm mass accuracy and resolution routinely in excess of 5000. Unique and error tolerant identification of yeast proteins as well as the sequencing of a novel protein illustrate the potential of the approach. The high data quality in tandem mass spectra and the additional information provided by the isotopic end labeling of peptides enabled automated interpretation of the spectra via simple software algorithms. The technique demonstrated here removes one of the last obstacles to routine and high throughput protein sequencing by mass spectrometry.

  9. Comparison of triple quadrupole, hybrid linear ion trap triple quadrupole, time-of-flight and LTQ-Orbitrap mass spectrometers in drug discovery phase metabolite screening and identification in vitro--amitriptyline and verapamil as model compounds.

    Science.gov (United States)

    Rousu, Timo; Herttuainen, Jukka; Tolonen, Ari

    2010-04-15

    Liquid chromatography in combination with mass spectrometry (LC/MS) is a superior analytical technique for metabolite profiling and identification studies performed in drug discovery and development laboratories. In the early phase of drug discovery the analytical approach should be both time- and cost-effective, thus providing as much data as possible with only one visit to the laboratory, without the need for further experiments. Recent developments in mass spectrometers have created a situation where many different mass spectrometers are available for the task, each with their specific strengths and drawbacks. We compared the metabolite screening properties of four main types of mass spectrometers used in analytical laboratories, considering both the ability to detect the metabolites and provide structural information, as well as the issues related to time consumption in laboratory and thereafter in data processing. Human liver microsomal incubations with amitriptyline and verapamil were used as test samples, and early-phase 'one lab visit only' approaches were used with all instruments. In total, 28 amitriptyline and 69 verapamil metabolites were found and tentatively identified. Time-of-flight mass spectrometry (TOFMS) was the only approach detecting all of them, shown to be the most suitable instrument for elucidating as comprehensive metabolite profile as possible leading also to lowest overall time consumption together with the LTQ-Orbitrap approach. The latter however suffered from lower detection sensitivity and false negatives, and due to slow data acquisition rate required slower chromatography. Approaches with triple quadrupole mass spectrometry (QqQ) and hybrid linear ion trap triple quadrupole mass spectrometry (Q-Trap) provided the highest amount of fragment ion data for structural elucidation, but, in addition to being unable to produce very high-important accurate mass data, they suffered from many false negatives, and especially with the Qq

  10. Shotgun Lipidomics by Sequential Precursor Ion Fragmentation on a Hybrid Quadrupole Time-of-Flight Mass Spectrometer

    Directory of Open Access Journals (Sweden)

    Brigitte Simons

    2012-02-01

    Full Text Available Shotgun lipidomics has evolved into a myriad of multi-dimensional strategies for molecular lipid characterization, including bioinformatics tools for mass spectrum interpretation and quantitative measurements to study systems-lipidomics in complex biological extracts. Taking advantage of spectral mass accuracy, scan speed and sensitivity of improved quadrupole linked time-of-flight mass analyzers, we developed a bias-free global lipid profiling acquisition technique of sequential precursor ion fragmentation called MS/MSALL. This generic information-independent tandem mass spectrometry (MS technique consists of a Q1 stepped mass isolation window through a set mass range in small increments, fragmenting and recording all product ions and neutral losses. Through the accurate MS and MS/MS information, the molecular lipid species are resolved, including distinction of isobaric and isomeric species, and composed into more precise lipidomic outputs. The method demonstrates good reproducibility and at least 3 orders of dynamic quantification range for isomeric ceramides in human plasma. More than 400 molecular lipids in human plasma were uncovered and quantified in less than 12 min, including acquisitions in both positive and negative polarity modes. We anticipate that the performance of sequential precursor ion fragmentation both in quality and throughput will lead to the uncovering of new avenues throughout the biomedical research community, enhance biomarker discovery and provide novel information target discovery programs as it will prospectively shed new insight into affected metabolic and signaling pathways.

  11. Increasing throughput and information content for in vitro drug metabolism experiments using ultra-performance liquid chromatography coupled to a quadrupole time-of-flight mass spectrometer.

    Science.gov (United States)

    Castro-Perez, Jose; Plumb, Robert; Granger, Jennifer H; Beattie, Iain; Joncour, Karine; Wright, Andrew

    2005-01-01

    The field of drug metabolism has been revolutionized by liquid chromatography/mass spectrometry (LC/MS) applications with new technologies such as triple quadrupoles, ion traps and time-of-flight (ToF) instrumentation. Over the years, these developments have often relied on the improvements to the mass spectrometer hardware and software, which has allowed users to benefit from lower levels of detection and ease-of-use. One area in which the development pace has been slower is in high-performance liquid chromatography (HPLC). In the case of metabolite identification, where there are many challenges due to the complex nature of the biological matrices and the diversity of the metabolites produced, there is a need to obtain the most accurate data possible. Reactive or toxic metabolites need to be detected and identified as early as possible in the drug discovery process, in order to reduce the very costly attrition of compounds in late-phase development. High-resolution, exact mass measurement plays a very important role in metabolite identification because it allows the elimination of false positives and the determination of non-trivial metabolites in a much faster throughput environment than any other standard current methodology available to this field. By improving the chromatographic resolution, increased peak capacity can be achieved with a reduction in the number of co-eluting species leading to superior separations. The overall enhancement in the chromatographic resolution and peak capacity is transferred into a net reduction in ion suppression leading to an improvement in the MS sensitivity. To investigate this, a number of in vitro samples were analyzed using an ultra-performance liquid chromatography (UPLC) system, with columns packed with porous 1.7 mum particles, coupled to a hybrid quadrupole time-of-flight (ToF) mass spectrometer. This technique showed very clear examples for fundamental gains in sensitivity, chromatographic resolution and speed of

  12. Screening for DNA adducts by data-dependent constant neutral loss-triple stage mass spectrometry with a linear quadrupole ion trap mass spectrometer.

    Science.gov (United States)

    Bessette, Erin E; Goodenough, Angela K; Langouët, Sophie; Yasa, Isil; Kozekov, Ivan D; Spivack, Simon D; Turesky, Robert J

    2009-01-15

    A two-dimensional linear quadrupole ion trap mass spectrometer (LIT/MS) was employed to simultaneously screen for DNA adducts of environmental, dietary, and endogenous genotoxicants, by data-dependent constant neutral loss scanning followed by triple-stage mass spectrometry (CNL-MS3). The loss of the deoxyribose (dR) from the protonated DNA adducts ([M + H - 116]+) in the MS/MS scan mode triggered the acquisition of MS3 product ion spectra of the aglycone adducts [BH2]+. Five DNA adducts of the tobacco carcinogen 4-aminobiphenyl (4-ABP) were detected in human hepatocytes treated with 4-ABP, and three DNA adducts of the cooked-meat carcinogen 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MeIQx) were identified in the livers of rats exposed to MeIQx, by the CNL-MS3 scan mode. Buccal cell DNA from tobacco smokers was screened for DNA adducts of various classes of carcinogens in tobacco smoke including 4-ABP, 2-amino-9H-pyrido[2,3-b]indole (AalphaC), and benzo[a]pyrene (BaP); the cooked-meat carcinogens MeIQx, AalphaC, and 2-amino-1-methyl-6-phenylmidazo[4,5-b]pyridine (PhIP); and the lipid peroxidation products acrolein (AC) and trans-4-hydroxynonenal (HNE). The CNL-MS3 scanning technique can be used to simultaneously screen for multiple DNA adducts derived from different classes of carcinogens, at levels of adduct modification approaching 1 adduct per 108 unmodified DNA bases, when 10 microg of DNA is employed for the assay.

  13. Analysis of psychoactive substances in water by information dependent acquisition on a hybrid quadrupole time-of-flight mass spectrometer.

    Science.gov (United States)

    Andrés-Costa, María Jesús; Andreu, Vicente; Picó, Yolanda

    2016-08-26

    Emerging drugs of abuse, belonging to many different chemical classes, are attracting users with promises of "legal" highs and easy access via internet. Prevalence of their consumption and abuse through wastewater-based epidemiology can only be realized if a suitable analytical screening procedure exists to detect and quantify them in water. Solid-phase extraction and ultra-high performance liquid chromatography quadrupole time-of-flight-mass spectrometry (UHPLC-QqTOF-MS/MS) was applied for rapid suspect screening as well as for the quantitative determination of 42 illicit drugs and metabolites in water. Using this platform, we were able to identify amphetamines, tryptamines, piperazines, pyrrolidinophenones, arylcyclohexylamines, cocainics, opioids and cannabinoids. Additionally, paracetamol, carbamazepine, ibersartan, valsartan, sulfamethoxazole, terbumeton, diuron, etc. (including degradation products as 3-hydroxy carbamazepine or deethylterbuthylazine) were detected. This method encompasses easy sample preparation and rapid identification of psychoactive drugs against a database that cover more than 2000 compounds that ionized in positive mode, and possibility to identify metabolites and degradation products as well as unknown compounds. The method for river water, influent and effluents samples was fully validated for the target psychoactive substances including assessment of matrix effects (-88-67.8%), recovery (42-115%), precision (psychoactive drugs biomarkers and other water contaminants is demonstrated.

  14. Mass spectrometers: instrumentation

    Science.gov (United States)

    Cooks, R. G.; Hoke, S. H., II; Morand, K. L.; Lammert, S. A.

    1992-09-01

    Developments in mass spectrometry instrumentation over the past three years are reviewed. The subject is characterized by an enormous diversity of designs, a high degree of competition between different laboratories working with either different or similar techniques and by extremely rapid progress in improving analytical performance. Instruments can be grouped into genealogical charts based on their physical and conceptual interrelationships. This is illustrated using mass analyzers of different types. The time course of development of particular instrumental concepts is illustrated in terms of the s-curves typical of cell growth. Examples are given of instruments which are at the exponential, linear and mature growth stages. The prime examples used are respectively: (i) hybrid instruments designed to study reactive collisions of ions with surfaces: (ii) the Paul ion trap; and (iii) the triple quadrupole mass spectrometer. In the area of ion/surface collisions, reactive collisions such as hydrogen radical abstraction from the surface by the impinging ion are studied. They are shown to depend upon the chemical nature of the surface through the use of experiments which utilize self-assembled monolayers as surfaces. The internal energy deposited during surface-induced dissociation upon collision with different surfaces in a BEEQ instrument is also discussed. Attention is also given to a second area of emerging instrumentation, namely technology which allows mass spectrometers to be used for on-line monitoring of fluid streams. A summary of recent improvements in the performance of the rapidly developing quadrupole ion trap instrument illustrates this stage of instrument development. Improvements in resolution and mass range and their application to the characterization of biomolecules are described. The interaction of theory with experiment is illustrated through the role of simulations of ion motion in the ion trap. It is emphasized that mature instruments play a

  15. Negative chemiions formed in jet fuel combustion: new insights from jet engine and laboratory measurements using a quadrupole ion trap mass spectrometer apparatus

    Energy Technology Data Exchange (ETDEWEB)

    Kiendler, A.; Aberle, S.; Arnold, F. [Max Planck Institute for Nuclaear Physics, Heidelberg (Germany). Atmospheric Physics Div.

    2000-07-01

    Measurements were made of mass numbers and composition of negative chemiions produced in jet fuel combustion in the exhaust of a jet engine and of a burner in the laboratory. The measurements made by a novel quadrupole ion trap mass spectrometer apparatus revealed the presence of three major ion families: ions containing an HSO{sub 4}{sup -} ''core's' or an NO{sub 3}{sup -} ''core's' and {sup O}HC-ions{sup .} The latter which contain C and H atoms and in part also 0 atoms can be divided into two subfamilies with even and odd mass numbers. It is proposed that the O HC ions are formed by free-electron attachment to HC and OHC molecules and/or ion-molecule reactions of primary negative chemiions with HC and OHC molecules. It is also proposed that HSO{sub 4}{sup -}- and NO{sub 3}{sup -}- containing ions are formed by ion-molecule reactions involving OHC ions and the sulfur- and reactive nitrogen-containing molecules H{sub 2}SO{sub 4}, SO{sub 3} and NO, NO{sub 2}, HNO{sub 2}, HNO{sub 3}. (author)

  16. Structure of coal: new approaches to characterizing organonitrogen and organosulfur functionalities in coal and coal liquids. Final report. [Finnigan triple quadrupole mass spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Cooks, R.G.

    1983-01-01

    This report describes the application of tandem mass spectrometry (MS/MS) to the analysis of coal-related materials. A Finnigan Triple State Quadrupole mass spectrometer was used for most of the results obtained in this study. Both collision energy (0 to 30 eV) and collision gas pressure (0 to 2.5 mtorr, typically argon) have significant effects on the spectra. Increasing the collision energy or collision pressure results in an increased fragmentation of the selected ion. The analytical utility of different chemical ionization (CI) reagent gases is shown. The MS/MS spectra of a selected ion obtained by isobutane and ammonia CI are identical, which paves the way for development of MS/MS libraries. A library is being developed especially for the analysis of coal-related materials. Three principal MS/MS scan modes (daughter, parent and neutral loss) are utilized in the analysis of coal-related materials. Parent and neutral loss scans characterize the complex mixture for particular chemical moieties (functional groups, structure type), while daughter scans are used for identification of specific components. SRC II was the principal sample studied by CI. Laser desorption methodology for coal analysis was developed. Other fuel-related materials were examined to generalize the analytical methodology being developed for the coal-related materials, including shale oil and diesel exhaust particulates. 35 references, 50 figures, 3 tables.

  17. Multiple and sequential data acquisition method: an improved method for fragmentation and detection of cross-linked peptides on a hybrid linear trap quadrupole Orbitrap Velos mass spectrometer.

    Science.gov (United States)

    Rudashevskaya, Elena L; Breitwieser, Florian P; Huber, Marie L; Colinge, Jacques; Müller, André C; Bennett, Keiryn L

    2013-02-05

    The identification and validation of cross-linked peptides by mass spectrometry remains a daunting challenge for protein-protein cross-linking approaches when investigating protein interactions. This includes the fragmentation of cross-linked peptides in the mass spectrometer per se and following database searching, the matching of the molecular masses of the fragment ions to the correct cross-linked peptides. The hybrid linear trap quadrupole (LTQ) Orbitrap Velos combines the speed of the tandem mass spectrometry (MS/MS) duty circle with high mass accuracy, and these features were utilized in the current study to substantially improve the confidence in the identification of cross-linked peptides. An MS/MS method termed multiple and sequential data acquisition method (MSDAM) was developed. Preliminary optimization of the MS/MS settings was performed with a synthetic peptide (TP1) cross-linked with bis[sulfosuccinimidyl] suberate (BS(3)). On the basis of these results, MSDAM was created and assessed on the BS(3)-cross-linked bovine serum albumin (BSA) homodimer. MSDAM applies a series of multiple sequential fragmentation events with a range of different normalized collision energies (NCE) to the same precursor ion. The combination of a series of NCE enabled a considerable improvement in the quality of the fragmentation spectra for cross-linked peptides, and ultimately aided in the identification of the sequences of the cross-linked peptides. Concurrently, MSDAM provides confirmatory evidence from the formation of reporter ions fragments, which reduces the false positive rate of incorrectly assigned cross-linked peptides.

  18. Comprehensive lipidome analysis by shotgun lipidomics on a hybrid quadrupole-orbitrap-linear ion trap mass spectrometer

    DEFF Research Database (Denmark)

    Almeida, Reinaldo; Pauling, Josch Konstantin; Sokol, Elena

    2015-01-01

    , including its high resolution power unsurpassed by any other contemporary Orbitrap instrumentation, its dynamic quantification range and its efficacy for in-depth structural characterization of molecular lipid species by quadrupole-based higher-energy collisional dissociation (HCD), and ion trap...... of fragmentation analysis demonstrated that combined use of HCD and CID yields complementary fragment ions of molecular lipid species. To support global lipidome analysis, we designed a method, termed MS(ALL), featuring high resolution FTMS analysis for lipid quantification, and FTMS(2) analysis using both HCD...... and CID and ITMS(3) analysis utilizing dual CID for in-depth structural characterization of molecular glycerophospholipid species. The performance of the MS(ALL) method was benchmarked in a comparative analysis of mouse cerebellum and hippocampus. This analysis demonstrated extensive lipidome...

  19. Comprehensive analysis of a multidimensional liquid chromatography mass spectrometry dataset acquired on a quadrupole selecting, quadrupole collision cell, time-of-flight mass spectrometer: I. How much of the data is theoretically interpretable by search engines?

    Science.gov (United States)

    Chalkley, Robert J; Baker, Peter R; Hansen, Kirk C; Medzihradszky, Katalin F; Allen, Nadia P; Rexach, Michael; Burlingame, Alma L

    2005-08-01

    An in-depth analysis of a multidimensional chromatography-mass spectrometry dataset acquired on a quadrupole selecting, quadrupole collision cell, time-of-flight (QqTOF) geometry instrument was carried out. A total of 3269 CID spectra were acquired. Through manual verification of database search results and de novo interpretation of spectra 2368 spectra could be confidently determined as predicted tryptic peptides. A detailed analysis of the non-matching spectra was also carried out, highlighting what the non-matching spectra in a database search typically are composed of. The results of this comprehensive dataset study demonstrate that QqTOF instruments produce information-rich data of which a high percentage of the data is readily interpretable.

  20. Isotopic Composition of Carbon Dioxide Released from Confidence Hills Sediment as Measured by the Sample Analysis at Mars (SAM) Quadrupole Mass Spectrometer

    Science.gov (United States)

    Franz, H. B.; Mahaffy, P. R.; Stern, J.; Archer, P., Jr.; Conrad, P.; Eigenbrode, J.; Freissinet, C.; Glavin, D.; Grotzinger, J. P.; Jones, J.; Ming, D.; McAdam, A.; Morris, R.; Navarro-Gozalez, R.; Owen, T.; Steele, A.; Summons, R.; Sutter, B.; Webster, C. R.

    2015-01-01

    In October 2014, the Mars Science Laboratory (MSL) "Curiosity" rover drilled into the sediment at the base of Mount Sharp in a location namsed Cionfidence Hills (CH). CH marked the fifth sample pocessed by the Sample Analysis at Mars (SAM) instrument suite since Curiosity arrived in Gale Crater, with previous analyses performed at Rocknest (RN), John Klein (JK), Cumberland (CB), and Windjana (WJ). Evolved gas analysis (EGA) of all samples has indicated H2O as well as O-, C- and S-bearing phases in the samples, often at abundances that would be below the detection limit of the CheMin instrument. By examining the temperatures at which gases are evolved from samples, SAM EGA data can help provide clues to the mineralogy of volatile-bearing phases when their identities are unclear to CheMin. SAM may also detect gases evolved from amorphous material in solid samples, which is not suitable for analysis by CheMin. Finally, the isotopic composition of these gases may suggest possible formation scenarios and relationships between phases. We will discuss C isotope ratios of CO2 evolved from the CH sample as measured with SAM's quadrupole mass spectrometer (QMS) and draw comparisons to samples previously analyzed by SAM.

  1. Quantitation of isobaric phosphatidylcholine species in human plasma using a hybrid quadrupole linear ion trap mass spectrometer

    Science.gov (United States)

    Phosphatidylcholine (PC) species in human plasma are used as biomarkers of disease. PC biomarkers are often limited by the inability to separate isobaric PC. In this work, we developed a targeted shotgun approach for analysis of isobaric and isomeric PC. This approach is comprised of two mass spectr...

  2. Characterization of TATP gas phase product ion chemistry via isotope labeling experiments using ion mobility spectrometry interfaced with a triple quadrupole mass spectrometer.

    Science.gov (United States)

    Tomlinson-Phillips, Jill; Wooten, Alfred; Kozole, Joseph; Deline, James; Beresford, Pamela; Stairs, Jason

    2014-09-01

    Identification of the fragment ion species associated with the ion reaction mechanism of triacetone triperoxide (TATP), a homemade peroxide-based explosive, is presented. Ion mobility spectrometry (IMS) has proven to be a key analytical technique in the detection of trace explosive material. Unfortunately, IMS alone does not provide chemical identification of the ions detected; therefore, it is unknown what ion species are actually formed and separated by the IMS. In IMS, ions are primarily characterized by their drift time, which is dependent on the ion׳s mass and molecular cross-section; thus, IMS as a standalone technique does not provide structural signatures, which is in sharp contrast to the chemical and molecular information that is generally obtained from other customary analytical techniques, such as NMR, Raman and IR spectroscopy and mass spectrometry. To help study the ion chemistry that gives rise to the peaks observed in IMS, the hardware of two different commercial IMS instruments has been directly coupled to triple quadrupole (QQQ) mass spectrometers, in order to ascertain each ion׳s corresponding mass/charge (m/z) ratios with different dopants at two temperatures. Isotope labeling was then used to help identify and confirm the molecular identity of the explosive fragment and adduct ions of TATP. The m/z values and isotope labeling experiments were used to help propose probable molecular formulas for the ion fragments. In this report, the fragment and adduct ions m/z 58 and 240 of TATP have been confirmed to be [C3H6NH·H](+) and [TATP·NH4](+), respectively; while the fragment ions m/z 73 and 89 of TATP are identified as having the molecular formulas [C4H9NH2](+) and [C4H9O2](+), respectively. It is anticipated that the work in this area will not only help to facilitate improvements in mobility-based detection (IMS and MS), but also aid in the development and optimization of MS-based detection algorithms for TATP.

  3. Accretion disks around a mass with quadrupole

    CERN Document Server

    Abishev, Medeu; Quevedo, Hernando; Toktarbay, Saken

    2015-01-01

    We consider the stability properties of test particles moving along circular orbits around a mass with quadrupole. We show that the quadrupole modifies drastically the properties of an accretion disk made of such test particles.

  4. Accretion disks around a mass with quadrupole

    Science.gov (United States)

    Abishev, M.; Boshkayev, K.; Quevedo, H.; Toktarbay, S.

    We consider the stability properties of circular orbits of test particles moving around a mass with quadrupole. We show that the quadrupole modifies drastically the properties of an accretion disk made of such test particles.

  5. Monitoring quinolone antibacterial residues in bovine tissues: extraction with hot water and liquid chromatography coupled to a single- or triple-quadrupole mass spectrometer.

    Science.gov (United States)

    Bogialli, Sara; D'Ascenzo, Giuseppe; Di Corcia, Antonio; Innocenti, Giorgiana; Laganà, Aldo; Pacchiarotta, Tiziana

    2007-01-01

    A rapid and sensitive procedure for determining residues of seven quinolone antibacterials in bovine muscle, kidney and liver is presented. The method is based on the matrix solid-phase dispersion (MSPD) technique with hot water as extractant followed by liquid chromatography/single quadrupole mass spectrometry (LC/MS) or triple-quadrupole mass spectrometry (LC/MS/MS). After dispersing tissue samples on hydrazine sulfate treated sand, target compounds were eluted from the MSPD column by passing through it 4 mL of water heated at 100 degrees C. After pH adjustment and filtration, 200 and 5 microL of the aqueous extracts were respectively injected into the LC/MS and LC/MS/MS instruments. With the former instrument, MS data were acquired in the three-ion selected ion monitoring mode, while MS/MS data acquisition was performed in the multi-reaction monitoring mode by selecting two precursor ion to product ion transitions for each target compound. Hot water appeared to be an efficient extracting medium, since absolute recoveries of the analytes were 84-102%. Using norfloxacin (a quinolone not used in veterinary medicine) as surrogate internal standard, the accuracy of the method at three concentration levels equal to 0.5, 1 and 1.5 times the maximum residue limits (MRLs) set by the european union was 88-109% with relative standard deviations (RSDs) not higher than 7%. The use of LC/MS/MS allowed detection and quantification of the analytes in any tissue considered to be performed at concentrations by far lower than half of their MRLs. Vice versa, the single-quadrupole MS arrangement, while succeeding in monitoring quinolones in muscle tissue at the 0.5 MRL level, showed to be not sufficiently selective for unambiguous identification of some quinolones in kidney and liver.

  6. Improved Mass Spectrometer Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The Improved Mass Spectrometer project will develop system requirements and analyze the path to space qualification.   The results of this project...

  7. Miniaturised TOF mass spectrometer

    Science.gov (United States)

    Rohner, U.; Wurz, P.; Whitby, J.

    2003-04-01

    For the BepiColombo misson of ESA to Mercury, we built a prototype of a miniaturised Time of Flight mass spectrometer with a low mass and low power consumption. Particles will be set free form the surface and ionized by short laser pluses. The mass spectrometer is dedicated to measure the elemental and isotopic composition of almost all elements of Mercurys planetary surface with an adequate dynamique range, mass range and mass resolution. We will present first results of our prototype and future designs.

  8. A micromachined mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Petzold, G.; Siebert, P.; Mueller, J. [Technische Univ. Hamburg-Harburg, Hamburg (Germany). Dept. of Microsystemtechnology

    2001-07-01

    This paper presents the concept, the processing and the simulated and measured characteristics of a miniaturised mass spectrometer, with dimensions of approximately only a few cm{sup 3}. The mass spectrometer consists of three main parts to be manufactured by micro structuring: an electron source, an ionisation chamber including accelerating and focusing units and a mass analyser with detector. Its fabrication is based on techniques used in micro-system processing and in particular anisotropic etching, thin film deposition, electroplating, and anodic bonding. The aim of the concept for this micro mass spectrometer is not only to scale down a macroscopic system but it also takes advantage of the added features of a micro system, i.e. a high Knudsen number of about 3 at a pressure of a few Pascal, and high field strengths at a relatively low voltage. Therefore, the demands on the vacuum systems and the electrical circuits are much more simple compared to a macroscopic mass spectrometer. In the presented design of the micro mass spectrometer the resolution is in the range of 10 to 20 at a sensitivity of several tens of ppm. (orig.)

  9. Confirmatory analysis of sulfonamide antibacterials in bovine liver and kidney: extraction with hot water and liquid chromatography coupled to a single- or triple-quadrupole mass spectrometer.

    Science.gov (United States)

    Bogialli, Sara; Curini, Roberta; Di Corcia, Antonio; Nazzari, Manuela; Sergi, Manuel

    2003-01-01

    A simple, specific, and rapid confirmatory method for determining 12 sulfonamide (SAs) antibacterials in bovine liver and kidney is presented. This method is based on the matrix solid-phase dispersion technique with hot water as extractant followed by liquid chromatography/mass spectrometry (LC/MS) with an electrospray ion source. The method was tailored for use with both single-quadrupole MS (I) and triple-quadrupole MS (II) instruments. After acidification and filtration of the aqueous extract, a 250-microL aliquot was injected into instrument I while only 25 microL was analyzed by instrument II. With instrument I MS data acquisition was performed in the selected ion monitoring (SIM) mode, selecting at least three ions for each target compound. With instrument II the selected reaction monitoring (SRM) mode with three fragmentation reactions for each compound was chosen. With the exception of sulfaquinoxaline (SQX), recovery of the analytes at the 50 ppb level in both liver and kidney was 72-96% with relative standard deviations (RSDs) ranging between 3 and 11%. The very poor recovery of SQX was due to its rapid enzymatic oxidation when in contact with the two tissues. With instrument I, limits of quantification (LOQs, S/N = 10) were 5-14 ppb of SAs. Even lower LOQs (1-8 ppb) were estimated by using instrument II, even though the extract volume analyzed was ten times lower than that with instrument I. With both matrices and using instrument I, severe ion signal suppression was experienced for the early-eluted SAs when trying to fractionate analytes by using a short chromatographic run time. This effect was traced to polar endogenous co-extractives eluted in the first part of the chromatographic run that interfered with gas-phase ion formation for SAs. Adopting more selective chromatographic conditions minimized this effect.

  10. Advanced stored waveform inverse Fourier transform technique for a matrix-assisted laser desorption/ionization quadrupole ion trap mass spectrometer.

    Science.gov (United States)

    Doroshenko, V M; Cotter, R J

    1996-01-01

    The stored waveform inverse Fourier transform (SWIFT) technique is used for broadband excitation of ions in an ion-trap mass spectrometer to perform mass-selective accumulation, isolation, and fragmentation of peptide ions formed by matrix-assisted laser desorption/ionization. Unit mass resolution is achieved for isolation of ions in the range of m/z up to 1300 using a two-step isolation technique with stretched-in-time narrow band SWIFT pulses at the second stage. The effect of 'stretched-in-time' waveforms is similar to that observed previously for mass-scan-rate reduction. The asymmetry phenomenon resulting from the stretched ion-trap electrode geometry is observed during application of normal and time-reversed waveforms and is similar to the asymmetry effects observed for forward and reverse mass scans in the resonance ejection mode. Mass-selective accumulation of ions from multiple laser shots was accomplished using a method described earlier that involves increasing the trapping voltage during ion introduction for more efficient trapping of ions.

  11. Development of a sensitive method for the determination of acrylamide in coffee using high-performance liquid chromatography coupled to a hybrid quadrupole Orbitrap mass spectrometer.

    Science.gov (United States)

    Pugajeva, Iveta; Jaunbergs, Janis; Bartkevics, Vadims

    2015-01-01

    The emerging trend towards high-resolution mass spectrometry (MS) alternatives was evaluated by the application of Orbitrap MS for the determination of acrylamide in coffee samples. The high resolving power of the Orbitrap MS provided the high selectivity and sensitivity that enabled quantitative analysis of acrylamide in complex matrices, such as coffee. Several sample preparation methods and scanning modes of the MS (full MS, t-SIM, t-MS2) were assessed in order to optimise parameters of the analytical method. The final procedure involved the extraction of acrylamide with acetonitrile, solid-phase extraction with dispersive primary secondary amine (PSA) and amino columns, and the detection by ultra-performance liquid chromatography coupled to a hybrid quadrupole-Orbitrap MS (HPLC-Q-Orbitrap) operated in targeted MS2 scanning mode. The repeatability of the method at the lowest calibration level (10 μg kg(-1)), expressed as relative standard deviation, was 7.8% and the average recovery of acrylamide was 111%. The proposed method was applied to the determination of acrylamide in 22 samples of roasted coffee obtained from the Latvian retail market. Acrylamide concentration in coffee samples was in the range of 166-503 μg kg(-1).

  12. In Situ Mass Spectrometer Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The In Situ Mass Spectrometer projects focuses on a specific subsystem to leverage advanced research for laser-based in situ mass spectrometer development...

  13. Core shell stationary phases for a novel separation of triglycerides in plant oils by high performance liquid chromatography with electrospray-quadrupole-time of flight mass spectrometer.

    Science.gov (United States)

    La Nasa, Jacopo; Ghelardi, Elisa; Degano, Ilaria; Modugno, Francesca; Colombini, Maria Perla

    2013-09-20

    A new method for the analysis of triglycerides (TAGs) in vegetable oils was developed using a Poroshell 120 EC-C18 column (3.0 mm×50 mm, 2.7 μm) with a high resolution ESI-Q-ToF tandem mass spectrometer as detection system. We used an Agilent Poroshell column, which is characterized by a recently developed stationary phase based on non-porous core particles. The results highlighted the advantages of this column in terms of the dramatic improvement in the number of theoretical plates and in low column backpressure. The developed method enabled us to analyze complex mixtures of more than 40 TAGs within less than 25 min and with a low backpressure (lower than 100 bar), and represents the first application of a core-shell stationary phase in reverse phase HPLC using an ESI-Q-ToF as detection system. The method was optimized on standards of TAGs, validated and applied to several plant oils. By a quantitative point of view, the method showed a very good linearity (r(2)>0.999) in the range 0.1-2.4 μg/g; high intra- and inter-day precision both in terms of retention times (RSD%<0.04%) and peak areas (RSD%<0.3%). Limits of detection and quantitation were lower than 0.03 μg/g and 0.10 μg/g, respectively.

  14. P202-S Expanding the Capabilities of Peptide MRM-Based Assays in Plasma Using a Hybrid Triple-Quadrupole Linear Ion-Trap Mass Spectrometer

    OpenAIRE

    Hunter, C.

    2007-01-01

    As the study of protein biomarkers increases in importance, technical limitations to the detection of low-abundance proteins and high-throughput, high-precision quantitation remain to be overcome. The complexity and dynamic range of the plasma proteome makes the task of specific, quantitative detection even more challenging. Multiple reaction monitoring (MRM) capabilities of triple quadrupole MS systems have been explored as solutions to this challenge due to their well-known sensitivity and ...

  15. MASS SPECTROMETER LEAK

    Science.gov (United States)

    Shields, W.R.

    1960-10-18

    An improved valve is described for precisely regulating the flow of a sample fluid to be analyzed, such as in a mass spectrometer, where a gas sample is allowed to "leak" into an evacuated region at a very low, controlled rate. The flow regulating valve controls minute flow of gases by allowing the gas to diffuse between two mating surfaces. The structure of the valve is such as to prevent the corrosive feed gas from contacting the bellows which is employed in the operation of the valve, thus preventing deterioration of the bellows.

  16. Exploring the human leukocyte phosphoproteome using a microfluidic reversed-phase-TiO2-reversed-phase high-performance liquid chromatography phosphochip coupled to a quadrupole time-of-flight mass spectrometer.

    Science.gov (United States)

    Raijmakers, Reinout; Kraiczek, Karsten; de Jong, Ad P; Mohammed, Shabaz; Heck, Albert J R

    2010-02-01

    The study of protein phosphorylation events is one of the most important challenges in proteome analysis. Despite the importance of phosphorylation for many regulatory processes in cells and many years of phosphoprotein and phosphopeptide research, the identification and characterization of phosphorylation by mass spectrometry is still a challenging task. Recently, we introduced an approach that facilitates the analysis of phosphopeptides by performing automated, online, TiO(2) enrichment of phosphopeptides prior to mass spectrometry (MS) analysis. The implementation of that method on a "plug-and-play" microfluidic high-performance liquid chromatography (HPLC) chip design will potentially open up efficient phosphopeptide enrichment methods enabling phosphoproteomics analyses by a broader research community. Following our initial proof of principle, whereby the device was coupled to an ion trap, we now show that this so-called phosphochip is capable of the enrichment of large numbers of phosphopeptides from complex cellular lysates, which can be more readily identified when coupled to a higher resolution quadrupole time-of-flight (Q-TOF) mass spectrometer. We use the phosphochip-Q-TOF setup to explore the phosphoproteome of nonstimulated primary human leukocytes where we identify 1012 unique phosphopeptides corresponding to 960 different phosphorylation sites providing for the first time an overview of the phosphoproteome of these important circulating white blood cells.

  17. Determination of selected pharmaceuticals in tap water and drinking water treatment plant by high-performance liquid chromatography-triple quadrupole mass spectrometer in Beijing, China.

    Science.gov (United States)

    Cai, Mei-Quan; Wang, Rong; Feng, Li; Zhang, Li-Qiu

    2015-02-01

    A simultaneous determination method of 14 multi-class pharmaceuticals using solid-phase extraction (SPE) followed by high-performance liquid chromatography-tandem mass spectrometer (HPLC-MS/MS) was established to measure the occurrence and distribution of these pharmaceuticals in tap water and a drinking water treatment plant (DWTP) in Beijing, China. Target compounds included seven anti-inflammatory drugs, two antibacterial drugs, two lipid regulation drugs, one antiepileptic drug, and one hormone. Limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.01 to 1.80 ng/L and 0.05 to 3.00 ng/L, respectively. Intraday and inter-day precisions, recoveries of different matrices, and matrix effects were also investigated. Of the 14 pharmaceutical compounds selected, nine were identified in tap water of Beijing downtown with the concentration up to 38.24 ng/L (carbamazepine), and the concentration levels of detected pharmaceuticals in tap water (water and finished water at the concentration ranged from 0.10 to 16.23 and 0.13 to 17.17 ng/L, respectively. Five compounds were detected most frequently in DWTP, namely antipyrine, carbamazepine, isopropylantipyrine, aminopyrine, and bezafibrate. Ibuprofen was found to be the highest concentration pharmaceutical during DWTP, up to 53.30 ng/L. DWTP shows a positive effect on the removal of most pharmaceuticals with 81.2-99.5 % removal efficiencies, followed by carbamazepine with 55.4 % removal efficiency, but it has no effect for removing ibuprofen and bezafibrate.

  18. A novel approach for identification of biologically active phenolic compounds in complex matrices using hybrid quadrupole-orbitrap mass spectrometer: A promising tool for testing antimicrobial activity of hops.

    Science.gov (United States)

    Dušek, Martin; Jandovská, Vladimíra; Čermák, Pavel; Mikyška, Alexandr; Olšovská, Jana

    2016-08-15

    The phenolic compounds, secondary metabolites of hops represent a large family of compounds that could be subsequently divided into smaller groups based on the similarities between their chemical structures. The antibacterial, antifungal and antiviral properties of hops are well known, but there is a lack of information about antimicrobial activities of individual hop compounds. This study was carried out with an objective to identify compounds present in hops that have potential antibacterial activity. In the first stage of experiment, the active compounds with potential anti-microbial activity had to be extracted from hop cones. Therefore, minced hop cones were applied on solid growth medium inoculated with Staphylococcus aureus. The active substances that migrated into the medium created an inhibition zone. In the second stage of experiment, the inhibition zones were cut out from Petri dishes, active compounds were extracted from these zones and consequently analyzed using LC-HRMS. These complex assays were developed and optimized. The data were acquired by using a quadrupole-orbitrap hybrid mass spectrometer by targeted-MS2 experiment in both ionization modes. The MS method has been developed as a screening method with a subsequent fragmentation of compound of interest on the base of inclusion mass list. The unknown compounds extracted from inhibition zones have been identified either by searching against a database or their structure has been elucidated on the basis of their fragmentation spectra. On the basis of this experiment the list of active compounds with potential anti-microbial activities was enhanced.

  19. A Bench Top Quadrupole Mass Spectrometer System for Accurate Analysis of Trace Noble Gas%准确分析微量惰性气体的轻便四极杆质谱系统

    Institute of Scientific and Technical Information of China (English)

    张子斌; Adolf.Goetz; 韦冠一; 李雪松; H.Gerken; 常永福

    2004-01-01

    A Bench top Quadrupole Mass Spectrometer System for Accurate Analysis of Trace Noble Gas was introduced in this paper. The inlet system was a especially designed one. And a capacitance pressure gauge with its linearity less than 0.01% was used to measure the fixed volume sample ratio. By using the calibration gas with the uncertainty of which less than 0.1% ,isotope condensed diluent could be quantified online. The procedure is done by alternate online mixture gas measurement of diluent gas, calibration gas to quantify the diluent gas, and diluent gas, sample gas to quantify the sample gas. The precision of six inlet from the same sample is +_0.13%0; The precision of six getting sample from the same source is less than ±0.5%. Self test was done by testing the mixture gas got with weighing method, in which consists Kr and Xe of 30 mg/kg. The system uncertainty tested to be below ±1%.

  20. A versatile computer-controlled pulsed nuclear quadrupole resonance spectrometer

    Science.gov (United States)

    Fisher, Gregory; MacNamara, Ernesto; Santini, Robert E.; Raftery, Daniel

    1999-12-01

    A new, pulsed nuclear quadrupole resonance (NQR) spectrometer capable of performing a variety of pulsed and swept experiments is described. The spectrometer features phase locked, superheterodyne detection using a commercial spectrum analyzer and a fully automatic, computer-controlled tuning and matching network. The tuning and matching network employs stepper motors which turn high power air gap capacitors in a "moving grid" optimization strategy to minimize the reflected power from a directional coupler. In the duplexer circuit, digitally controlled relays are used to switch different lengths of coax cable appropriate for the different radio frequencies. A home-built pulse programmer card controls the timing of radio frequency pulses sent to the probe, while data acquisition and control software is written in Microsoft Quick Basic. Spin-echo acquisition experiments are typically used to acquire the data, although a variety of pulse sequences can be employed. Scan times range from one to several hours depending upon the step resolution and the spectral range required for each experiment. Pure NQR spectra of NaNO2 and 3-aminopyridine are discussed.

  1. Qualitative and quantitative analysis of the chemical constituents in Mahuang-Fuzi-Xixin decoction based on high performance liquid chromatography combined with time-of-flight mass spectrometry and triple quadrupole mass spectrometers.

    Science.gov (United States)

    Sun, Qihui; Cao, Hongjie; Zhou, Yanyan; Wang, Xu; Jiang, Haiqiang; Gong, Lili; Yang, Yong; Rong, Rong

    2016-11-01

    High-performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-TOF/MS) and high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-QQQ/MS/MS) were utilized to clarify the chemical constituents of Mahuang-Fuzi-Xixin Decoction. There are 52 compounds, including alkaloids, amino acids and organic acids were identified or tentatively characterized by their characteristic high resolution mass data by HPLC-QQQ/MS/MS. In the subsequent quantitative analysis, 10 constituents, including methyl ephedrine, aconine, songrine, fuziline, neoline, talatisamine, chasmanine, benzoylmesaconine, benzoylaconine and benzoylhypaconine were simultaneously determined by HPLC-QQQ/MS/MS with multiple reaction monitoring mode. Satisfactory linearity was achieved with wide linear range and fine determination coefficient (r > 0.9992). The relative standard deviations (RSD) of inter- and intra-day precisions were chemical constituents studying, including identification and quantification of Mahuang-Fuzi-Xixin decoction. Copyright © 2016 John Wiley & Sons, Ltd.

  2. Electron Transfer Dissociation of All Ions at All Times, MSETD, in a Quadrupole Time-of-Flight (Q-ToF) Mass Spectrometer

    Science.gov (United States)

    Cramer, Christian N.; Brown, Jeffery M.; Tomczyk, Nick; Nielsen, Peter Kresten; Haselmann, Kim F.

    2016-12-01

    Data-independent mass spectral acquisition is particularly powerful when combined with ultra-performance liquid chromatography (LC) that provides excellent separation of most components present in a given sample. Data-independent analysis (DIA) consists of alternating full MS scans and scans with fragmentation of all ions within a selected m/z range, providing precursor masses and structure information, respectively. Fragmentation spectra are acquired either by sequential isolation and fragmentation of sliding m/z ranges or fragmenting all ions entering the MS instrument with no ion isolation, termed broadband DIA. Previously, broadband DIA has only been possible using collision induced dissociation (CID). Here, we report the use of electron transfer dissociation (ETD) as the fragmentation technique in broadband DIA instead of traditional collision induced dissociation (CID) during MSE. In this approach, which we refer to as MSETD, we implement the inherent benefits provided by ETD, such as discrimination of leucine and isoleucine, in a DIA setup. The combination of DIA analysis and ETD fragmentation with supplemental CID energy provides a powerful platform to obtain information on all precursors and their sequence from a single experiment.

  3. Electron Transfer Dissociation of All Ions at All Times, MSETD, in a Quadrupole Time-of-Flight (Q-ToF) Mass Spectrometer

    Science.gov (United States)

    Cramer, Christian N.; Brown, Jeffery M.; Tomczyk, Nick; Nielsen, Peter Kresten; Haselmann, Kim F.

    2017-02-01

    Data-independent mass spectral acquisition is particularly powerful when combined with ultra-performance liquid chromatography (LC) that provides excellent separation of most components present in a given sample. Data-independent analysis (DIA) consists of alternating full MS scans and scans with fragmentation of all ions within a selected m/z range, providing precursor masses and structure information, respectively. Fragmentation spectra are acquired either by sequential isolation and fragmentation of sliding m/z ranges or fragmenting all ions entering the MS instrument with no ion isolation, termed broadband DIA. Previously, broadband DIA has only been possible using collision induced dissociation (CID). Here, we report the use of electron transfer dissociation (ETD) as the fragmentation technique in broadband DIA instead of traditional collision induced dissociation (CID) during MSE. In this approach, which we refer to as MSETD, we implement the inherent benefits provided by ETD, such as discrimination of leucine and isoleucine, in a DIA setup. The combination of DIA analysis and ETD fragmentation with supplemental CID energy provides a powerful platform to obtain information on all precursors and their sequence from a single experiment.

  4. Multi-Pass Quadrupole Mass Analyzer

    Science.gov (United States)

    Prestage, John D.

    2013-01-01

    Analysis of the composition of planetary atmospheres is one of the most important and fundamental measurements in planetary robotic exploration. Quadrupole mass analyzers (QMAs) are the primary tool used to execute these investigations, but reductions in size of these instruments has sacrificed mass resolving power so that the best present-day QMA devices are still large, expensive, and do not deliver performance of laboratory instruments. An ultra-high-resolution QMA was developed to resolve N2 +/CO+ by trapping ions in a linear trap quadrupole filter. Because N2 and CO are resolved, gas chromatography columns used to separate species before analysis are eliminated, greatly simplifying gas analysis instrumentation. For highest performance, the ion trap mode is used. High-resolution (or narrow-band) mass selection is carried out in the central region, but near the DC electrodes at each end, RF/DC field settings are adjusted to allow broadband ion passage. This is to prevent ion loss during ion reflection at each end. Ions are created inside the trap so that low-energy particles are selected by low-voltage settings on the end electrodes. This is beneficial to good mass resolution since low-energy particles traverse many cycles of the RF filtering fields. Through Monte Carlo simulations, it is shown that ions are reflected at each end many tens of times, each time being sent back through the central section of the quadrupole where ultrahigh mass filtering is carried out. An analyzer was produced with electrical length orders of magnitude longer than its physical length. Since the selector fields are sized as in conventional devices, the loss of sensitivity inherent in miniaturizing quadrupole instruments is avoided. The no-loss, multi-pass QMA architecture will improve mass resolution of planetary QMA instruments while reducing demands on the RF electronics for high-voltage/high-frequency production since ion transit time is no longer limited to a single pass. The

  5. Influence of instrumental parameters on the kinetic energy of ions and plasma temperature for a hexapole collision/reaction-cell-based inductively coupled plasma quadrupole mass spectrometer.

    Science.gov (United States)

    Favre, Georges; Brennetot, René; Chartier, Frédéric; Tortajada, Jeanine

    2009-02-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in inorganic analytical chemistry for element and/or isotope ratio measurements. The presence of interferences, which is one of the main limitations of this method, has been addressed in recent years with the introduction of collision/reaction cell devices on ICP-MS apparatus. The study of ion-molecule reactions in the gas phase then became of great importance for the development of new analytical strategies. Knowing the kinetic energy and the electronic states of the ions prior to their entrance into the cell, i.e., just before they react, thereby constitutes crucial information for the interpretation of the observed reactivities. Such studies on an ICP-MS commonly used for routine analyses require the determination of the influence of different instrumental parameters on the energy of the ions and on the plasma temperature from where ions are sampled. The kinetic energy of ions prior to their entrance into the cell has been connected to the voltage applied to the hexapole according to a linear relationship determined from measurements of ion energy losses due to collisions with neutral gas molecules. The effects of the plasma forward power, sampling depth, and the addition of a torch shield to the ICP source were then examined. A decrease of the plasma potential due to the torch shielding, already mentioned in the literature, has been quantified in this study at about 3 V.

  6. Mass spectrometric analysis of the marine lipophilic biotoxins pectenotoxin-2 and okadaic acid by four different types of mass spectrometers

    NARCIS (Netherlands)

    Gerssen, A.; Mulder, P.P.J.; Rhijn, van J.A.; Boer, de J.

    2008-01-01

    The performances of four different mass spectrometers [triple-quadrupole (TQ), time-of-flight (ToF), quadrupole ToF (Q-ToF) and ion trap (IT)] for the detection of the marine lipophilic toxins pectenotoxin-2 (PTX2) and okadaic acid (OA) were investigated. The spectral data obtained with the differen

  7. A hybrid liquid chromatography-mass spectrometry strategy in a forensic laboratory for opioid, cocaine and amphetamine classes in human urine using a hybrid linear ion trap-triple quadrupole mass spectrometer.

    Science.gov (United States)

    Dowling, Geraldine; Regan, Liam; Tierney, Julie; Nangle, Michael

    2010-10-29

    A rapid method has been developed to analyse morphine, codeine, morphine-3-glucuronide, 6-monoacetylmorphine, cocaine, benzoylegonine, buprenorphine, dihydrocodeine, cocaethylene, 3,4-methylenedioxyamphetamine, ketamine, 3,4-methylenedioxymethamphetamine, pseudoephedrine, lignocaine, benzylpiperazine, methamphetamine, amphetamine, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine and methadone in human urine. Urine samples were diluted with methanol:water (1:1, v/v) and sample aliquots were analysed by hybrid linear ion trap-triple quadrupole mass spectrometry with a runtime of 12.5 min. Multiple reaction monitoring (MRM) as survey scan and an enhanced product ion (EPI) scan as dependent scan were performed in an information-dependent acquisition (IDA) experiment. Finally, drug identification and confirmation was carried out by library search with a developed in-house MS/MS library based on EPI spectra at a collision energy spread of 35±15 in positive mode and MRM ratios. The method was validated in urine, according to the criteria defined in Commission Decision 2002/657/EC. At least two MRM transitions for each substance were monitored in addition to EPI spectra and deuterated analytes were used as internal standards for quantitation. The reporting level was 0.05 μg mL(-1) for the range of analytes tested. The regression coefficients (r(2)) for the calibration curves (0-4 μg mL(-1)) in the study were ≥0.98. The method proved to be simple and time efficient and was implemented as an analytical strategy for the illicit drug monitoring of opioids, cocaines and amphetamines in criminal samples from crime offenders, abusers or victims in the Republic of Ireland. To the best of our knowledge there are no hybrid LC-MS applications using MRM mode and product ion spectra in the linear ion trap mode for opioids, cocaines or amphetamines with validation data in urine.

  8. Imaging mass spectrometer with mass tags

    Science.gov (United States)

    Felton, James S.; Wu, Kuang Jen J.; Knize, Mark G.; Kulp, Kristen S.; Gray, Joe W.

    2013-01-29

    A method of analyzing biological material by exposing the biological material to a recognition element, that is coupled to a mass tag element, directing an ion beam of a mass spectrometer to the biological material, interrogating at least one region of interest area from the biological material and producing data, and distributing the data in plots.

  9. Pulsed spectrometer for nuclear quadrupole resonance for remote detection of nitrogen in explosives

    Science.gov (United States)

    Anferov, V. P.; Mozjoukhine, G. V.; Fisher, R.

    2000-04-01

    We describe a pulsed spectrometer for detection of nuclear quadrupole resonance on the nuclei of nitrogen N-14 with fast Fourier transform. The use of a multipulse sequence, four channel system for data registration and processing permits detection of the nuclear quadrupole resonance (NQR) signal in the presence of strong interference and the piezo effect. Using this spectrometer we registered the NQR signal from an explosive sample of 150 g (92% RDX) at a distance of 22 cm, and the time of detection was 81 s.

  10. Advanced Mass Spectrometers for Hydrogen Isotope Analyses

    Energy Technology Data Exchange (ETDEWEB)

    Chastagner, P.

    2001-08-01

    This report is a summary of the results of a joint Savannah River Laboratory (SRL) - Savannah River Plant (SRP) ''Hydrogen Isotope Mass Spectrometer Evaluation Program''. The program was undertaken to evaluate two prototype hydrogen isotope mass spectrometers and obtain sufficient data to permit SRP personnel to specify the mass spectrometers to replace obsolete instruments.

  11. Acquisition of HPLC-Mass Spectrometer

    Science.gov (United States)

    2015-08-18

    31-Jan-2015 Approved for Public Release; Distribution Unlimited Final Report: Acquisition of HPLC -Mass Spectrometer The views, opinions and/or findings...published in peer-reviewed journals: Final Report: Acquisition of HPLC -Mass Spectrometer Report Title The acquisition of the mass spectrometer has been a

  12. New schemes of static mass spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Baisanov, O.A. [Military Institute of Air Defense Forces, Aktobe (Kazakhstan); Doskeyev, G.A. [Aktobe State University named after K. Zhubanov, Aktobe (Kazakhstan); Spivak-Lavrov, I.F., E-mail: baisanov@mail.ru [Aktobe State University named after K. Zhubanov, Aktobe (Kazakhstan)

    2011-07-21

    Different possibilities to increase the 'quality', or Q-quantity, of static mass spectrometers by expanding the ion beam before it enters the magnetic field are analyzed. The design of mass spectrometers using a cone-shaped achromatic prism is discussed. Different variants of achromatic mass spectrometers using electrostatic prisms and sector magnetic fields are also considered.

  13. DC superconducting quantum interference device usable in nuclear quadrupole resonance and zero field nuclear magnetic spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Non Q. (San Diego, CA); Clarke, John (Berkeley, CA)

    1993-01-01

    A spectrometer for measuring the nuclear quadrupole resonance spectra or the zero-field nuclear magnetic resonance spectra generated by a sample is disclosed. The spectrometer uses an amplifier having a dc SQUID operating in a flux-locked loop for generating an amplified output as a function of the intensity of the signal generated by the sample. The flux-locked loop circuit includes an integrator. The amplifier also includes means for preventing the integrator from being driven into saturation. As a result, the time for the flux-locked loop to recover from the excitation pulses generated by the spectrometer is reduced.

  14. DC superconducting quantum interference device usable in nuclear quadrupole resonance and zero field nuclear magnetic spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Fan, N.Q.; Clarke, J.

    1993-10-19

    A spectrometer for measuring the nuclear quadrupole resonance spectra or the zero-field nuclear magnetic resonance spectra generated by a sample is disclosed. The spectrometer uses an amplifier having a dc SQUID operating in a flux-locked loop for generating an amplified output as a function of the intensity of the signal generated by the sample. The flux-locked loop circuit includes an integrator. The amplifier also includes means for preventing the integrator from being driven into saturation. As a result, the time for the flux-locked loop to recover from the excitation pulses generated by the spectrometer is reduced. 7 figures.

  15. High-Resolution Mass Spectrometers

    Science.gov (United States)

    Marshall, Alan G.; Hendrickson, Christopher L.

    2008-07-01

    Over the past decade, mass spectrometry has been revolutionized by access to instruments of increasingly high mass-resolving power. For small molecules up to ˜400 Da (e.g., drugs, metabolites, and various natural organic mixtures ranging from foods to petroleum), it is possible to determine elemental compositions (CcHhNnOoSsPp…) of thousands of chemical components simultaneously from accurate mass measurements (the same can be done up to 1000 Da if additional information is included). At higher mass, it becomes possible to identify proteins (including posttranslational modifications) from proteolytic peptides, as well as lipids, glycoconjugates, and other biological components. At even higher mass (˜100,000 Da or higher), it is possible to characterize posttranslational modifications of intact proteins and to map the binding surfaces of large biomolecule complexes. Here we review the principles and techniques of the highest-resolution analytical mass spectrometers (time-of-flight and Fourier transform ion cyclotron resonance and orbitrap mass analyzers) and describe some representative high-resolution applications.

  16. A computer controlled mass spectrometer system for investigating the decomposition of non-metallic materials under atmospheric conditions

    Science.gov (United States)

    Thompson, J. M.

    1985-01-01

    A PDP 11/23 quadrupole mass spectrometer system was coupled to a nondiscriminating gas inlet system permitting gases at atmospheric pressure to be admitted into a high vacuum chamber containing the ion source of the mass spectrometer without separation of the gaseous components. The resolution of related software problems has resulted in a convenient computer-mass spectrometer system capable of generating masses, relative intensities and related data on the gaseous products resulting from the atmospheric thermal decomposition of nonmetallic materials.

  17. A computer controlled mass spectrometer system for investigating the decomposition of non-metallic materials under atmospheric conditions

    Science.gov (United States)

    Thompson, J. M.

    1985-01-01

    A PDP 11/23 quadrupole mass spectrometer system was coupled to a nondiscriminating gas inlet system permitting gases at atmospheric pressure to be admitted into a high vacuum chamber containing the ion source of the mass spectrometer without separation of the gaseous components. The resolution of related software problems has resulted in a convenient computer-mass spectrometer system capable of generating masses, relative intensities and related data on the gaseous products resulting from the atmospheric thermal decomposition of nonmetallic materials.

  18. Quantitative analysis of antiretroviral drugs in lysates of peripheral blood mononuclear cells using MALDI-triple quadrupole mass spectrometry.

    NARCIS (Netherlands)

    Kampen, JJ van; Burgers, P.C.; Gruters, R.A.; Osterhaus, A.D.; Groot, R. de; Luider, T.M.; Volmer, D.A.

    2008-01-01

    We report here on the use of a prototype matrix-assisted laser desorption/ionization (MALDI)-triple quadrupole mass spectrometer for quantitative analysis of six antiretroviral drugs in lysates of peripheral blood mononuclear cells (PBMC). Of the five investigated MALDI matrixes, 2,5-dihydroxybenzoi

  19. A Mass Spectrometer Simulator in Your Computer

    Science.gov (United States)

    Gagnon, Michel

    2012-01-01

    Introduced to study components of ionized gas, the mass spectrometer has evolved into a highly accurate device now used in many undergraduate and research laboratories. Unfortunately, despite their importance in the formation of future scientists, mass spectrometers remain beyond the financial reach of many high schools and colleges. As a result,…

  20. Preliminary results from LADEE's Neutral Mass Spectrometer (NMS)

    Science.gov (United States)

    Benna, Mehdi; Mahaffy, Paul; Hodges, Richard

    2014-05-01

    The Neutral Mass Spectrometer (NMS) of the Lunar Atmosphere and Dust Environment Explorer (LADEE) Mission is a high sensitivity quadrupole mass spectrometer designed to measure the composition and variability of the tenuous lunar atmosphere. The instrument has been observing the lunar exosphere since 10/17/2013, initially from a near circular 250 km altitude orbit and since 11/11/2013 from an elliptical orbit that reaches to 30-60 km altitude near the sunrise terminator. During its first four months in orbit, the NMS instrument successfully detected exospheric helium, argon and neon and mapped their spatial and temporal variability. Furthermore, the NMS instrument was able to establish new upper limits for many other exospheric species either sputtered or thermally evolved from the lunar surface. This talk will summarize these preliminary results from the NMS measurements.

  1. Calibration Techniques for Triple Quadrupole Gas Chromatography-Mass Spectrometer%三重四级杆气相色谱-串联质谱联用仪的校准

    Institute of Scientific and Technical Information of China (English)

    赵迎晨; 冯帅博; 李琛; 李佳

    2016-01-01

    The calibration method of GC–MS/MS instrument was discussed. The calibration items such as resolution, qualitative and quantitative repeatability, detection limit, quality accuracy and spectral library search were proposed referring to JJF1164 –2006 Calibration Specification for Bench Top Gas Chromatography–Mass Spectrometers. The method was used to calibrate GC–MS/MS and it is proved that the method is reasonable.%参考JJF 1164–2006《台式气相色谱–质谱联用仪校准规范》,探讨了三重四级杆气相色谱–串联质谱联用仪的校准方法,提出了以分辨力、定性定量重复性、检出限、质量准确性与谱库检索等5项作为相关校准项目。经验证,用该校准方法对三重四级杆气相色谱–串联质谱联用仪进行校准是可行的。

  2. Mass measurements on radioactive isotopes using the ISOLTRAP spectrometer

    CERN Document Server

    Dilling, J; Kluge, H J; Kohl, A; Lamour, E; Marx, G; Schwarz, S C; Bollen, G; Kellerbauer, A G; Moore, R B; Henry, S

    2000-01-01

    ISOLTRAP is a Penning trap mass spectrometer installed at the on line isotope separator ISOLDE at CERN. Direct measurements of the masses of short lived radio isotopes are performed using the existing triple trap system. This consists of three electromagnetic traps in tandem: a Paul trap to accumulate and bunch the 60 keV dc beam, a Penning trap for cooling and isobar separation, and a precision Penning trap for the determination of the masses by cyclotron resonance. Measurements of masses of unknown mercury isotopes and in the vicinity of doubly magic /sup 208/Pb are presented, all with an accuracy of delta m/m approximately=1*10/sup -7/. Developments to replace the Paul trap by a radiofrequency quadrupole ion guide system to increase the collection efficiency are presently under way and the status is presented. (10 refs).

  3. Low Power Mass Spectrometer employing TOF Project

    Data.gov (United States)

    National Aeronautics and Space Administration — A low power Mass Spectrometer employing multiple time of flight circuits for parallel processing is possible with a new innovation in design of the Time of flight...

  4. Mass Spectrometer for Airborne Micro-Organisms

    Science.gov (United States)

    Sinha, M. P.; Friedlander, S. K.

    1986-01-01

    Bacteria and other micro-organisms identified continously with aid of new technique for producing samples for mass spectrometer. Technique generates aerosol of organisms and feeds to spectrometer. Given species of organism produces characteristic set of peaks in mass spectrum and thereby identified. Technique useful for monitoring bacterial makeup in environmental studies and in places where cleanliness is essential, such as hospital operating rooms, breweries, and pharmaceutical plants.

  5. Mass Quadrupole as a Source of Naked Singularities

    CERN Document Server

    Quevedo, Hernando

    2010-01-01

    We investigate the gravitational field of a static mass with quadrupole moment in empty space. It is shown that in general this configuration is characterized by the presence of curvature singularities without a surrounding event horizon. These naked singularities generate an effective field of repulsive gravity which, in turn, drastically changes the behavior of test particles. As a possible consequence, the accretion disk around a naked singularity presents a particular discontinuous structure.

  6. Ion Mobility Spectrometer / Mass Spectrometer (IMS-MS).

    Energy Technology Data Exchange (ETDEWEB)

    Hunka, Deborah E; Austin, Daniel

    2005-10-01

    The use of Ion Mobility Spectrometry (IMS)in the Detection of Contraband Sandia researchers use ion mobility spectrometers for trace chemical detection and analysis in a variety of projects and applications. Products developed in recent years based on IMS-technology include explosives detection personnel portals, the Material Area Access (MAA) checkpoint of the future, an explosives detection vehicle portal, hand-held detection systems such as the Hound and Hound II (all 6400), micro-IMS sensors (1700), ordnance detection (2500), and Fourier Transform IMS technology (8700). The emphasis to date has been on explosives detection, but the detection of chemical agents has also been pursued (8100 and 6400).Combining Ion Mobility Spectrometry (IMS) with Mass Spectrometry (MS)The IMS-MS combination overcomes several limitations present in simple IMS systems. Ion mobility alone is insufficient to identify an unknown chemical agent. Collision cross section, upon which mobility is based, is not sufficiently unique or predictable a priori to be able to make a confident peak assignment unless the compounds present are already identified. Molecular mass, on the other hand, is much more readily interpreted and related to compounds. For a given compound, the molecular mass can be determined using a pocket calculator (or in one's head) while a reasonable value of the cross-section might require hours of computation time. Thus a mass spectrum provides chemical specificity and identity not accessible in the mobility spectrum alone. In addition, several advanced mass spectrometric methods, such as tandem MS, have been extensively developed for the purpose of molecular identification. With an appropriate mass spectrometer connected to an ion mobility spectrometer, these advanced identification methods become available, providing greater characterization capability.3 AcronymsIMSion mobility spectrometryMAAMaterial Access AreaMSmass spectrometryoaTOForthogonal acceleration time

  7. Ion mobility spectrometer / mass spectrometer (IMS-MS).

    Energy Technology Data Exchange (ETDEWEB)

    Hunka Deborah Elaine; Austin, Daniel E.

    2005-07-01

    The use of Ion Mobility Spectrometry (IMS) in the Detection of Contraband Sandia researchers use ion mobility spectrometers for trace chemical detection and analysis in a variety of projects and applications. Products developed in recent years based on IMS-technology include explosives detection personnel portals, the Material Area Access (MAA) checkpoint of the future, an explosives detection vehicle portal, hand-held detection systems such as the Hound and Hound II (all 6400), micro-IMS sensors (1700), ordnance detection (2500), and Fourier Transform IMS technology (8700). The emphasis to date has been on explosives detection, but the detection of chemical agents has also been pursued (8100 and 6400). Combining Ion Mobility Spectrometry (IMS) with Mass Spectrometry (MS) is described. The IMS-MS combination overcomes several limitations present in simple IMS systems. Ion mobility alone is insufficient to identify an unknown chemical agent. Collision cross section, upon which mobility is based, is not sufficiently unique or predictable a priori to be able to make a confident peak assignment unless the compounds present are already identified. Molecular mass, on the other hand, is much more readily interpreted and related to compounds. For a given compound, the molecular mass can be determined using a pocket calculator (or in one's head) while a reasonable value of the cross-section might require hours of computation time. Thus a mass spectrum provides chemical specificity and identity not accessible in the mobility spectrum alone. In addition, several advanced mass spectrometric methods, such as tandem MS, have been extensively developed for the purpose of molecular identification. With an appropriate mass spectrometer connected to an ion mobility spectrometer, these advanced identification methods become available, providing greater characterization capability.

  8. 用Bessel-Box型能量分析器的离子规和四极质谱计的性能%Performance of Ionization Gauge and Quadrupole Mass Spectrometer with Bessel-Box Type Energy Analyzer:a Review of Progress

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A novel energy analyzer with a simple-structured Bessel-box has been successfully developed and incorporated into ionization gauges and quadrupole mass spectrometers (QMS) to improve their measurement of the total and partial pressures,respectively.We found that the energy analyzer may not only effectively separate the gas phase ions and electron stimulated desorption (ESD) ions produced in the ionizer,but also screen the ion collector from irradiation of the soft X-rays and VUVphotons generated in the ionizer.The screening effects considerably better the trace impurity detection limit of the QMS down to a few tens ppb in the pressure range of 10-3 Pa.The modified ionization gauge is capable of measuring pressure ranging from 10-11 to 10-6 Pa in the pulse counting mode and its upper limit may extends to 10-3 Pa in DC ion current mode with typical sensitivities factor of(6.7±0.2)×10-3 Pa-1 for N2 and (2.3±0.2)×10-3 Pa-1 for H2,respectively.No ESD ions was observed in the simple-looking spectrum obtained with the modified QMS.We also found that the energy spectra of fragment ions depend strongly on species of parent ions.

  9. Multistage Fragmentation of Ion Trap Mass Spectrometry System and Pseudo-MS3 of Triple Quadrupole Mass Spectrometry Characterize Certain (E)-3-(Dimethylamino)-1-arylprop-2-en-1-ones: A Comparative Study

    OpenAIRE

    Ali S. Abdelhameed; Adnan A. Kadi; Abdel-Aziz, Hatem A.; Angawi, Rihab F.; Mohamed W. Attwa; Al-Rashood, Khalid A.

    2014-01-01

    A new approach was recently introduced to improve the structure elucidation power of tandem mass spectrometry simulating the MS3 of ion trap mass spectrometry system overcoming the different drawbacks of the latter. The fact that collision induced dissociation in the triple quadrupole mass spectrometer system provides richer fragment ions compared to those achieved in the ion trap mass spectrometer system utilizing resonance excitation. Moreover, extracting comprehensive spectra in the ion tr...

  10. Gas-dust-impact mass spectrometer

    CERN Document Server

    Semkin, N D; Myasnikov, S V; Pomelnikov, R A

    2002-01-01

    Paper describes design of a mass spectrometer to study element composition of micro meteorite and man-made particles in space. Paper describes a way to improve resolution of mass spectrometer based on variation of parameters of accelerating electric field in time. The advantage of the given design of mass spectrometer in comparison with similar ones is its large operating area and higher resolution at the comparable weight and dimensions. Application of a combined design both for particles and for gas enables to remove space vehicle degassing products from the spectrum and, thus, to improve reliability of the acquired information, as well as, to acquire information on a gas component of the external atmosphere of a space vehicle

  11. High-Precision Mass Measurements of Exotic Nuclei with the Triple-Trap Mass Spectrometer Isoltrap

    CERN Multimedia

    Blaum, K; Zuber, K T; Stanja, J

    2002-01-01

    The masses of close to 200 short-lived nuclides have already been measured with the mass spectrometer ISOLTRAP with a relative precision between 1$\\times$10$^{-7}$ and 1$\\times$10^{-8}$. The installatin of a radio-frequency quadrupole trap increased the overall efficiency by two orders of magnitude which is at present about 1%. In a recent upgrade, we installed a carbon cluster laser ion source, which will allow us to use carbon clusters as mass references for absolute mass measurements. Due to these improvements and the high reliability of ISOLTRAP we are now able to perform accurate high-precision mass measurements all over the nuclear chart. We propose therefore mass measurements on light, medium and heavy nuclides on both sides of the valley of stability in the coming four years. ISOLTRAP is presently the only instrument capable of the high precision required for many of the proposed studies.

  12. Portable Tandem Mass Spectrometer Analyzer

    Science.gov (United States)

    1991-07-01

    FILE : MHCI TUNE TABLE 84 (SCANNING with PARENT) SCAN RANGE 10.9 TO 700.0 TUNE MASS 355.0 (AUTO) >LENS 1-3 -13. 88 0. 2: POFF - 1. 2 9: COFF - 4. 1 3...electronics, and glass shops . 04- 0 4- CD IL - -- it * I ; CHAPTER 3 EXPERIMENTAL RESULTS AND SOURCE DEVELOPMENT Results with API Source Configuration

  13. Linear mass scans in quadrupole ion traps using the inverse Mathieu q scan.

    Science.gov (United States)

    Snyder, Dalton T; Pulliam, Christopher J; Cooks, R Graham

    2016-11-30

    Secular frequency scanning is a method of mass selectively scanning ions out of a quadrupole ion trap by linearly ramping the frequency of the resonance ejection signal through ion secular frequencies at constant rf amplitude and frequency. The method is electronically much simpler than resonance ejection but it requires a complex nonlinear calibration procedure to correlate mass-to-charge with time. A method of secular frequency scanning in quadrupole ion traps is described in which mass-to-charge is linear with time. This method, termed an "inverse Mathieu q scan", contrasts with linear frequency sweeping which requires a complex nonlinear mass calibration procedure. In the current method, mass scans are forced to be linear with time by scanning the frequency of the supplementary ac so that there is an inverse relationship between the ejected ion's Mathieu q parameter and time. In all cases, excellent mass spectral linearity is observed. The rf amplitude is shown to control both the scan range and the scan rate, whereas the ac amplitude and scan rate influence the mass resolution. The scan rate depends linearly on the rf amplitude, a unique feature of this scan. Although changes in either rf or ac amplitude affect the positions of peaks in time, they do not change the mass calibration procedure since this only requires a simple linear fit of m/z vs time. Space charge effects are shown to give rise to significant changes in resolution as well as to mass shifts. A method of secular frequency scanning which provides a linear mass scale has been demonstrated. The inverse Mathieu q scan offers a significant increase in mass range and power savings while maintaining access to linearity, paving the way for a mass spectrometer based completely on ac waveforms for ion isolation, ion activation, and ion ejection. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  14. Handheld miniature ion trap mass spectrometers.

    Science.gov (United States)

    Ouyang, Zheng; Noll, Robert J; Cooks, R Graham

    2009-04-01

    For field applications, "miniature" and "rapid" have become almost synonymous, yet these small mass spectrometers are not useful if performance is too severely compromised. (To listen to a podcast about this feature, please go to the Analytical Chemistry website at pubs.acs.org/journal/ancham .).

  15. Mass measurements with a Penning trap mass spectrometer at ISOLDE

    CERN Document Server

    Bollen, G; Audi, G; Beck, D; Herfurth, F; Kluge, H J; Kohl, A; Lunney, M D; Moore, R B; De Saint-Simon, M; Schark, E; Schwarz, S; Szerypo, J

    1998-01-01

    Penning trap mass measurements on radioactive isotopes are performed with the ISOLTRAP mass spectrometer at ISOLDE/CERN. In the last years the applicability of the spectrometer has been considerably extended. The most recent measurements were carried out on isotopes of rare earth elements and on isotopes with Z=80-85. An accuracy of $\\delta$ m/m approximately=1$\\cdot$10$^{-7}$was achieved. (19 refs).

  16. Validation of a qualitative screening method for pesticides in fruits and vegetables by gas chromatography quadrupole-time of flight mass spectrometry with atmospheric pressure chemical ionization

    NARCIS (Netherlands)

    Portoles, T.; Mol, J.G.J.; Sancho, J.V.; Lopez, F.J.; Hernandez, F.

    2014-01-01

    A wide-scope screening method was developed for the detection of pesticides in fruit and vegetables. The method was based on gas chromatography coupled to a hybrid quadrupole time-of-flight mass spectrometer with an atmospheric pressure chemical ionization source (GC-(APCI)QTOF MS). A non-target acq

  17. Quantitative determination of multi markers in five varieties of Withania somnifera using ultra-high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometer combined with multivariate analysis: Application to pharmaceutical dosage forms.

    Science.gov (United States)

    Chandra, Preeti; Kannujia, Rekha; Saxena, Ankita; Srivastava, Mukesh; Bahadur, Lal; Pal, Mahesh; Singh, Bhim Pratap; Kumar Ojha, Sanjeev; Kumar, Brijesh

    2016-09-10

    An ultra-high performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for simultaneous quantification of six major bioactive compounds in five varieties of Withania somnifera in various plant parts (leaf, stem and root). The analysis was accomplished on Waters ACQUITY UPLC BEH C18 column with linear gradient elution of water/formic acid (0.1%) and acetonitrile at a flow rate of 0.3mLmin(-1). The proposed method was validated with acceptable linearity (r(2), 0.9989-0.9998), precision (RSD, 0.16-2.01%), stability (RSD, 1.04-1.62%) and recovery (RSD ≤2.45%), under optimum conditions. The method was also successfully applied for the simultaneous determination of six marker compounds in twenty-six marketed formulations. Hierarchical cluster analysis and principal component analysis were applied to discriminate these twenty-six batches based on characteristics of the bioactive compounds. The results indicated that this method is advance, rapid, sensitive and suitable to reveal the quality of Withania somnifera and also capable of performing quality evaluation of polyherbal formulations having similar markers/raw herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Towards a universal product ion mass spectral library - reproducibility of product ion spectra across eleven different mass spectrometers.

    Science.gov (United States)

    Hopley, Chris; Bristow, Tony; Lubben, Anneke; Simpson, Alec; Bull, Elaine; Klagkou, Katerina; Herniman, Julie; Langley, John

    2008-06-01

    Product ion spectra produced by collision-induced dissociation (CID) in tandem mass spectrometry experiments can differ markedly between instruments. There have been a number of attempts to standardise the production of product ion spectra; however, a consensus on the most appropriate approach to the reproducible production of spectra has yet to be reached. We have previously reported the comparison of product ion spectra on a number of different types of instruments - a triple quadrupole, two ion traps and a Fourier transform ion cyclotron resonance mass spectrometer (Bristow AWT, Webb KS, Lubben AT, Halket JM. Rapid Commun. Mass Spectrom. 2004; 18: 1). The study showed that a high degree of reproducibility was achievable. The goal of this study was to improve the comparability and reproducibility of CID product ion mass spectra produced in different laboratories and using different instruments. This was carried out experimentally by defining a spectral calibration point on each mass spectrometer for product ion formation. The long-term goal is the development of a universal (instrument independent) product ion mass spectral library for the identification of unknowns. The spectra of 48 compounds have been recorded on eleven mass spectrometers: six ion traps, two triple quadrupoles, a hybrid triple quadrupole, and two quadrupole time-of-flight instruments. Initially, 4371 spectral comparisons were carried out using the data from eleven instruments and the degree of reproducibility was evaluated. A blind trial has also been carried out to assess the reproducibility of spectra obtained during LC/MS/MS. The results suggest a degree of reproducibility across all instrument types using the tuning point technique. The reproducibility of the product ion spectra is increased when comparing the tandem in time type instruments and the tandem in space instruments as two separate groups. This may allow the production of a more limited, yet useful, screening library for LC

  19. Research relative to an advanced rod control system for quadrupole mass spectrometry applications

    Science.gov (United States)

    Carignan, George R.

    1987-01-01

    The design of a suitable amplifier output stage using available transistors and passive components is summarized. All of the analysis and calculation confirm that it is feasible to design the amplifier and quadrupole coupling circuit needed for the Advanced Rod Control System. The progress obtained so far concerning the three frequency tank circuits to be used in the oscillator for the mass spectrometer of the Cometary Rendezvous Asteroid Flyby (CRAF) project is presented. Results from this study look promising. However, it is not known what minimum impedance levels are required to make it possible for the oscillator to work properly. Therefore, it is necessary to construct a prototype circuit in the laboratory which can be measured and tested in an oscillator circuit. Continued attempts will be made to develop a useful inductor motor with better characteristics than the one being used at the moment. It is important that such a model be found if computer simulation is to reflect reality more closely.

  20. Control Electronics for Air-Borne Quadrupole Ion Mass Spectrometer.

    Science.gov (United States)

    1981-10-01

    REMOVE ALL I DEFINITIONS CPI OD9H ;IS ENTRY A Y? JNZ GETALL ;ERROR IN ENTRY SRART AGAIN GI8 LXI H,M15 ;DISPLAY DATAVAL ? MESSAG MVI A, (18H CALL MESSAG...ASCII " BJC-2" MI AS5CI I " DATAVAL ?" MI6 ASCI I "DECIMAL?" ml ASCII "SUB IDS?" M1 ASCII "SUB ID#" M19 ASCII " LbYT LOC" M2U ASCii " II3YT LOC" M21

  1. Recent exploits of the ISOLTRAP mass spectrometer

    CERN Document Server

    Kreim, S; Naimi, S; Blaum, K; Breitenfeldt, M; Rossel, R E; Fink, D; Stanja, J; Atanasov, D; Borgmann, Ch; Cocolios, T E; Zuber, K; Wolf, R N; George, S; Neidherr, D; Nicol, T; Rosenbusch, M; Lunney, D; Boehm, Ch; Manea, V; Herlert, A; Koester, U; Beck, D; Wienholtz, F; Kellerbauer, A; Ramirez, E Minaya; Schweikhard, L

    2013-01-01

    The Penning-trap mass spectrometer ISOLTRAP, located at the isotope-separator facility ISOLDE (CERN), is presented in its current form taking into account technical developments since 2007. Three areas of developments are presented. The reference ion sources have been modified to guarantee a sufficient supply of reference ions for mass measurements and systematic studies. Different excitation schemes have been investigated for manipulation of the ion motion in the Penning trap, to enhance either the purification or measurement process. A multi-reflection time-of-flight mass separator has been implemented and can now be routinely used for purification and as a versatile tool for beam analysis. (C) 2013 Elsevier B.V. All rights reserved.

  2. High-throughput shotgun lipidomics by quadrupole time-of-flight mass spectrometry

    DEFF Research Database (Denmark)

    Ståhlman, Marcus; Ejsing, Christer S.; Tarasov, Kirill;

    2009-01-01

    Technological advances in mass spectrometry and meticulous method development have produced several shotgun lipidomic approaches capable of characterizing lipid species by direct analysis of total lipid extracts. Shotgun lipidomics by hybrid quadrupole time-of-flight mass spectrometry allows...

  3. [Determination of congo red in beef by high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry].

    Science.gov (United States)

    Lin, Hui; Xu, Chunxiang; Yan, Chunrong; Zhang, Zheng; Wang, Suilou

    2013-09-01

    A method was developed for the determination of congo red in beef. The analyte was identified by high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry (LC-QTOF MS) and quantitatively determined by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the congo red in the beef sample was separated on an Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HD UPLC column (50 mm x 2.1 mm, 1.8 microm) HPLC , using 95% (volume percentage) methanol as the mobile phase at 0.2 mL/min. The detection was performed on an AB 4000 + triple quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM) mode. The results showed that the linear range of congo red mass concentration was 0.03 - 1 mg/L with the correlation coefficient of 0.999 8. The method had a good precision with the RSDs lower than 5% and the recoveries ranging from 88% to 91%. The limit of detection (LOD) of congo red was 0.01 mg/L. With good reproducibility, the method is simple, fast and effective for the determination of the illegally added congo red in beef and other meat products.

  4. Miniaturised Time-of-Flight Mass Spectrometer

    Science.gov (United States)

    Rohner, U.; Benz, W.; Whitby, J. A.; Wurz, P.; Schulz, R.; Romstedt, J.

    2004-04-01

    Originally intended for the European Space Agency's BepiColombo mission to Mercury, we have built a series of highly miniaturised laser ablation time of flight mass spectrometers (LMS), suitable for in situ measurements of the elemental and isotopic composition of the surface of airless planetary bodies. The instruments will determine ma jor, minor, and trace element abundances in minerals on a spatial scale of 10 m, and will have sufficient dynamic range and mass resolution to perform useful isotopic measurements in favourable cases. Solid material is simultaneously evaporated and ionised by means of laser ablation, requiring intense pulsed laser radiation. Laser ablation was chosen as the sample introduction technique principally because of its high spatial resolution and the lack of any need for sample preparation. Advantages of the technique include simplicity of the resulting design, speed of measurement, and the ability for depth profiling (potentially important for a regolith in which mineral grains are coated with impact produced glass). Time of flight mass spectrometers are simple, robust devices that couple well to a pulsed ion source and we have previous experience of their construction for space flight, e.g. the ROSINA instrument suite for the ROSETTA mission. For BepiColombo, we have built two prototype instruments, one with a design mass of 500 g and a volume comparable to a beer can intended to be deployed on a static lander, and a smaller cigarettebox sized version with a design mass of 250 g, small enough to be integrated in a rover or robotic arm.

  5. Multistage fragmentation of ion trap mass spectrometry system and pseudo-MS3 of triple quadrupole mass spectrometry characterize certain (E)-3-(dimethylamino)-1-arylprop-2-en-1-ones: a comparative study.

    Science.gov (United States)

    Abdelhameed, Ali S; Kadi, Adnan A; Abdel-Aziz, Hatem A; Angawi, Rihab F; Attwa, Mohamed W; Al-Rashood, Khalid A

    2014-01-01

    A new approach was recently introduced to improve the structure elucidation power of tandem mass spectrometry simulating the MS(3) of ion trap mass spectrometry system overcoming the different drawbacks of the latter. The fact that collision induced dissociation in the triple quadrupole mass spectrometer system provides richer fragment ions compared to those achieved in the ion trap mass spectrometer system utilizing resonance excitation. Moreover, extracting comprehensive spectra in the ion trap needs multistage fragmentation, whereas similar fragment ions may be acquired from one stage product ion scan using the triple quadrupole mass spectrometer. The new strategy was proven to enhance the qualitative performance of tandem mass spectrometry for structural elucidation of different chemical entities. In the current study we are endeavoring to prove our hypothesis of the efficiency of the new pseudo-MS(3) technique via its comparison with the MS(3) mode of ion trap mass spectrometry system. Ten pharmacologically and synthetically important (E)-3-(dimethylamino)-1-arylprop-2-en-1-ones (enaminones 4a-j) were chosen as model compounds for this study. This strategy permitted rigorous identification of all fragment ions using triple quadrupole mass spectrometer with sufficient specificity. It can be used to elucidate structures of different unknown components. The data presented in this paper provide clear evidence that our new pseudo-MS(3) may simulate the MS(3) of ion trap spectrometry system.

  6. Multistage Fragmentation of Ion Trap Mass Spectrometry System and Pseudo-MS3 of Triple Quadrupole Mass Spectrometry Characterize Certain (E-3-(Dimethylamino-1-arylprop-2-en-1-ones: A Comparative Study

    Directory of Open Access Journals (Sweden)

    Ali S. Abdelhameed

    2014-01-01

    Full Text Available A new approach was recently introduced to improve the structure elucidation power of tandem mass spectrometry simulating the MS3 of ion trap mass spectrometry system overcoming the different drawbacks of the latter. The fact that collision induced dissociation in the triple quadrupole mass spectrometer system provides richer fragment ions compared to those achieved in the ion trap mass spectrometer system utilizing resonance excitation. Moreover, extracting comprehensive spectra in the ion trap needs multistage fragmentation, whereas similar fragment ions may be acquired from one stage product ion scan using the triple quadrupole mass spectrometer. The new strategy was proven to enhance the qualitative performance of tandem mass spectrometry for structural elucidation of different chemical entities. In the current study we are endeavoring to prove our hypothesis of the efficiency of the new pseudo-MS3 technique via its comparison with the MS3 mode of ion trap mass spectrometry system. Ten pharmacologically and synthetically important (E-3-(dimethylamino-1-arylprop-2-en-1-ones (enaminones 4a–j were chosen as model compounds for this study. This strategy permitted rigorous identification of all fragment ions using triple quadrupole mass spectrometer with sufficient specificity. It can be used to elucidate structures of different unknown components. The data presented in this paper provide clear evidence that our new pseudo-MS3 may simulate the MS3 of ion trap spectrometry system.

  7. Measurements of deuterium quadrupole coupling in propiolic acid and fluorobenzenes using pulsed-beam Fourier transform microwave spectrometers.

    Science.gov (United States)

    Sun, Ming; Sargus, Bryan A; Carey, Spencer J; Kukolich, Stephen G

    2015-04-21

    The pure rotational spectra of deuterated propiolic acids (HCCCOOD and DCCCOOH), 1-fluorobenzene (4-d1), and 1,2-difluorobenzene (4-d1) in their ground states have been measured using two Fourier transform microwave (FTMW) spectrometers at the University of Arizona. For 1-fluorobenzene (4-d1), nine hyperfine lines of three different ΔJ = 0 and 1 transitions were measured to check the synthesis method and resolution. For 1,2-difluorobenzene (4-d1), we obtained 44 hyperfine transitions from 1 to 12 GHz, including 14 different ΔJ = 0, 1 transitions. Deuterium quadrupole coupling constants along the three principal inertia axes were well determined. For deuterated propiolic acids, 37 hyperfine lines of Pro-OD and 59 hyperfine lines of Pro-CD, covering 11 and 12 different ΔJ = - 1, 0, 1 transitions, respectively, were obtained from 5 to 16 GHz. Deuterium quadrupole coupling constants along the three inertia axes were well resolved for Pro-OD. For Pro-CD, only eQq(aa) was determined due to the near coincidence of the CD bond and the least principal inertia axis. Some measurements were made using a newer FTMW spectrometer employing multiple free induction decays as well as background subtraction. For 1-fluorobenzene (4-d1) and 1,2-difluorobenzene (4-d1), a very large-cavity (1.2 m mirror dia.) spectrometer yielded very high resolution (2 kHz) spectra.

  8. Further development and application of a mobile multiple-reflection time-of-flight mass spectrometer for analytical high-resolution tandem mass spectrometry

    OpenAIRE

    Lippert, Wayne

    2016-01-01

    In this work, a mobile multiple-reflection time-of-flight mass spectrometer (MR-TOF-MS) for analytical mass spectrometry was enhanced in many important aspects. Technical as well as software-based improvements have been added to the instrument, thus greatly increasing its performance and applicability. Changes have been applied to the whole beam preparation system of the MR-TOF-MS. In this context, the electronic setup was completely overhauled and a quadrupole mass filter was commissioned. C...

  9. A novel aircraft-based tandem mass spectrometer for atmospheric ion and trace gas measurements

    Science.gov (United States)

    Moehler, O.; Reiner, Th.; Arnold, F.

    1993-05-01

    The general design and operation of a novel aircraft-based triple-quadrupole mass spectrometer (TQMS) developed for the improved detection and collisional analysis of atmospheric ions and trace gases are described. The instrument is also suitable for laboratory collision-induced dissociation measurements, studies of ion-molecule reactions, and analytical applications. Highly sensitive and selective trace gas detection by chemical ionization mass spectrometry is also possible using a novel ion injection technique. Result of aircraft-based measurements made with the TQMS are summarized.

  10. Low-frequency nuclear magnetic resonance and nuclear quadrupole resonance spectrometer based on a dc superconducting quantum interference device

    Science.gov (United States)

    Fan, N. Q.; Clarke, John

    1991-06-01

    A sensitive spectrometer, based on a dc superconducting quantum interference device, for the direct detection of low-frequency pulsed nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR), is described. The frequency response extends from about 10 to 200 kHz, and the recovery time after the magnetic pulse is removed is typically 50 μs. As examples, NMR spectra are shown from Pt and Cu metal powders in a magnetic field of 6 mT, and NQR spectra are shown from 2D in a tunneling methyl group and 14N in NH4ClO4.

  11. Improved ion optics for introduction of ions into a 9.4-T Fourier transform ion cyclotron resonance mass spectrometer.

    Science.gov (United States)

    Chen, Yu; Leach, Franklin E; Kaiser, Nathan K; Dang, Xibei; Ibrahim, Yehia M; Norheim, Randolph V; Anderson, Gordon A; Smith, Richard D; Marshall, Alan G

    2015-01-01

    Enhancements to the ion source and transfer optics of our 9.4 T Fourier transform ion cyclotron resonance (ICR) mass spectrometer have resulted in improved ion transmission efficiency for more sensitive mass measurement of complex mixtures at the MS and MS/MS levels. The tube lens/skimmer has been replaced by a dual ion funnel and the following octopole by a quadrupole for reduced ion cloud radial expansion before transmission into a mass-selective quadrupole. The number of ions that reach the ICR cell is increased by an order of magnitude for the funnel/quadrupole relative to the tube lens/skimmer/octopole. Copyright © 2015 John Wiley & Sons, Ltd.

  12. Quantification of sterol lipids in plants by quadrupole time-of-flight mass spectrometry

    Science.gov (United States)

    Wewer, Vera; Dombrink, Isabel; vom Dorp, Katharina; Dörmann, Peter

    2011-01-01

    Glycerolipids, sphingolipids, and sterol lipids constitute the major lipid classes in plants. Sterol lipids are composed of free and conjugated sterols, i.e., sterol esters, sterol glycosides, and acylated sterol glycosides. Sterol lipids play crucial roles during adaption to abiotic stresses and plant-pathogen interactions. Presently, no comprehensive method for sterol lipid quantification in plants is available. We used nanospray ionization quadrupole-time-of-flight mass spectrometry (Q-TOF MS) to resolve and identify the molecular species of all four sterol lipid classes from Arabidopsis thaliana. Free sterols were derivatized with chlorobetainyl chloride. Sterol esters, sterol glycosides, and acylated sterol glycosides were ionized as ammonium adducts. Quantification of molecular species was achieved in the positive mode after fragmentation in the presence of internal standards. The amounts of sterol lipids quantified by Q-TOF MS/MS were validated by comparison with results obtained with TLC/GC. Quantification of sterol lipids from leaves and roots of phosphate-deprived A. thaliana plants revealed changes in the amounts and molecular species composition. The Q-TOF method is far more sensitive than GC or HPLC. Therefore, Q-TOF MS/MS provides a comprehensive strategy for sterol lipid quantification that can be adapted to other tandem mass spectrometers. PMID:21382968

  13. STS-46 plasma composition measurements using the EOIM-3 mass spectrometer

    Science.gov (United States)

    Hunton, Donald E.; Trzcinski, Edmund; Gosselin, Roger; Koontz, Steven; Leger, Lubert; Visentine, James T.

    1995-01-01

    One of the active instruments incorporated into the Evaluation of Oxygen Interactions with Materials - 3 experiment was a quadrupole mass spectrometer. The primary objectives for this instrument, which was built by the Air Force Phillips Laboratory and was a veteran of the STS-4 flight in 1982, were to quantify the flux of atomic oxygen striking the test surfaces in the EOIM-3 payload and to detect surface reaction products from the materials in the carousel. Other speakers in this session have covered the results of these experiments. Prior to the 40-hour-long dedicated EOIM-3 mission segment at the end of the STS-46 flight, the authors used the mass spectrometer to make measurements of ion and neutral gas composition in the shuttle environment. About 25 hours of data were collected during a variety of mission events, including Eureca deployment at high altitude and many tethered satellite system operations.

  14. Fabrication and testing of the recoil mass spectrometer at Bombay Pelletron

    Indian Academy of Sciences (India)

    S Nagaraj; H C Jain; P K Joshi; S D Paul; R Palit; H V Panchal; B S Naidu; A Chatterjee; A Navin

    2001-07-01

    A recoil mass spectrometer (RMS) has been designed, fabricated and installed at the 15°S beam-line of the Pelletron at TIFR. The RMS consists of a quadrupole doublet just after the target chamber followed by an ‘electrostatic deflector’, a magnetic dipole and a second electrostatic deflector. The recoils produced in the 12C+58Ni reaction using 60 MeV 12C beam were focussed with the help of electric and magnetic fields and detected in a strip detector placed at the focal plane of the RMS. Further testing of the spectrometer to obtain mass resolution and efficiency are in progress.

  15. Development of a Compact Resonance Ionization Mass Spectrometer for Trace Element Analysis of Potassium

    CERN Document Server

    Iwata, Yoshihiro; Minowa, Makoto

    2010-01-01

    A compact resonance ionization mass spectrometer is developed using two laser diodes and a quadrupole mass spectrometer to perform trace element analysis of potassium. With the help of a narrow linewidth of the laser diode, the isotope shifts of $^{40}{\\rm K}$ and $^{41}{\\rm K}$ of the 405~nm line with respect to $^{39}{\\rm K}$, corresponding to the transition of $4\\,^2$S$_{1/2}\\rightarrow$ $5\\,^2$P$^\\circ_{1/2}$, are measured to be $207\\pm13$~MHz and $451\\pm10$~MHz, respectively, by comparing them to the known hyperfine splitting widths of the $4\\,^2{\\rm S}_{1/2}$ ground state of each potassium isotope. The overall detection efficiency of an order of $\\sim10^{-6}$ in our setup indicates the availability of RIMS to the analysis of the trace metal impurities on or in a certain material such as the contamination assessment of semiconductor wafers.

  16. Measurements of deuterium quadrupole coupling in propiolic acid and fluorobenzenes using pulsed-beam Fourier transform microwave spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Ming; Sargus, Bryan A.; Carey, Spencer J.; Kukolich, Stephen G., E-mail: kukolich@u.arizona.edu [Department of Chemistry and Biochemistry, University of Arizona, Tucson, Arizona 85721 (United States)

    2015-04-21

    The pure rotational spectra of deuterated propiolic acids (HCCCOOD and DCCCOOH), 1-fluorobenzene (4-d{sub 1}), and 1,2-difluorobenzene (4-d{sub 1}) in their ground states have been measured using two Fourier transform microwave (FTMW) spectrometers at the University of Arizona. For 1-fluorobenzene (4-d{sub 1}), nine hyperfine lines of three different ΔJ = 0 and 1 transitions were measured to check the synthesis method and resolution. For 1,2-difluorobenzene (4-d{sub 1}), we obtained 44 hyperfine transitions from 1 to 12 GHz, including 14 different ΔJ = 0, 1 transitions. Deuterium quadrupole coupling constants along the three principal inertia axes were well determined. For deuterated propiolic acids, 37 hyperfine lines of Pro-OD and 59 hyperfine lines of Pro-CD, covering 11 and 12 different ΔJ = − 1, 0, 1 transitions, respectively, were obtained from 5 to 16 GHz. Deuterium quadrupole coupling constants along the three inertia axes were well resolved for Pro-OD. For Pro-CD, only eQq{sub aa} was determined due to the near coincidence of the CD bond and the least principal inertia axis. Some measurements were made using a newer FTMW spectrometer employing multiple free induction decays as well as background subtraction. For 1-fluorobenzene (4-d{sub 1}) and 1,2-difluorobenzene (4-d{sub 1}), a very large-cavity (1.2 m mirror dia.) spectrometer yielded very high resolution (2 kHz) spectra.

  17. [Qualitative and quantitative analysis of amygdalin and its metabolite prunasin in plasma by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry].

    Science.gov (United States)

    Gao, Meng; Wang, Yuesheng; Wei, Huizhen; Ouyang, Hui; He, Mingzhen; Zeng, Lianqing; Shen, Fengyun; Guo, Qiang; Rao, Yi

    2014-06-01

    A method was developed for the determination of amygdalin and its metabolite prunasin in rat plasma after intragastric administration of Maxing shigan decoction. The analytes were identified by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and quantitatively determined by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the qualitative analysis of amygdalin and prunasin in the plasma sample was performed on a Shim-pack XR-ODS III HPLC column (75 mm x 2.0 mm, 1.6 microm), using acetonitrile-0.1% (v/v) formic acid aqueous solution. The detection was performed on a Triple TOF 5600 quadrupole time of flight mass spectrometer. The quantitative analysis of amygdalin and prunasin in the plasma sample was performed by separation on an Agilent C18 HPLC column (50 mm x 2.1 mm, 1.7 microm), using acetonitrile-0.1% (v/v) formic acid aqueous solution. The detection was performed on an AB Q-TRAP 4500 triple quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM) mode. The qualitative analysis results showed that amygdalin and its metabolite prunasin were detected in the plasma sample. The quantitative analysis results showed that the linear range of amygdalin was 1.05-4 200 ng/mL with the correlation coefficient of 0.999 0 and the linear range of prunasin was 1.25-2 490 ng/mL with the correlation coefficient of 0.997 0. The method had a good precision with the relative standard deviations (RSDs) lower than 9.20% and the overall recoveries varied from 82.33% to 95.25%. The limits of detection (LODs) of amygdalin and prunasin were 0.50 ng/mL. With good reproducibility, the method is simple, fast and effective for the qualitative and quantitative analysis of the amygdalin and prunasin in plasma sample of rats which were administered by Maxing shigan decoction.

  18. THOR Ion Mass Spectrometer instrument - IMS

    Science.gov (United States)

    Retinò, Alessandro; Kucharek, Harald; Saito, Yoshifumi; Fraenz, Markus; Verdeil, Christophe; Leblanc, Frederic; Techer, Jean-Denis; Jeandet, Alexis; Macri, John; Gaidos, John; Granoff, Mark; Yokota, Shoichiro; Fontaine, Dominique; Berthomier, Matthieu; Delcourt, Dominique; Kistler, Lynn; Galvin, Antoniette; Kasahara, Satoshi; Kronberg, Elena

    2016-04-01

    Turbulence Heating ObserveR (THOR) is the first mission ever flown in space dedicated to plasma turbulence. Specifically, THOR will study how turbulent fluctuations at kinetic scales heat and accelerate particles in different turbulent environments within the near-Earth space. To achieve this goal, THOR payload is being designed to measure electromagnetic fields and particle distribution functions with unprecedented resolution and accuracy. Here we present the Ion Mass Spectrometer (IMS) instrument that will measure the full three-dimensional distribution functions of near-Earth main ion species (H+, He+, He++ and O+) at high time resolution (~ 150 ms for H+ , ~ 300 ms for He++) with energy resolution down to ~ 10% in the range 10 eV/q to 30 keV/q and angular resolution ~ 10°. Such high time resolution is achieved by mounting multiple sensors around the spacecraft body, in similar fashion to the MMS/FPI instrument. Each sensor combines a top-hat electrostatic analyzer with deflectors at the entrance together with a time-of-flight section to perform mass selection. IMS electronics includes a fast sweeping high voltage board that is required to make measurements at high cadence. Ion detection includes Micro Channel Plates (MCP) combined with Application-Specific Integrated Circuits (ASICs) for charge amplification, discrimination and time-to-digital conversion (TDC). IMS is being designed to address many of THOR science requirements, in particular ion heating and acceleration by turbulent fluctuations in foreshock, shock and magnetosheath regions. The IMS instrument is being designed and will be built by an international consortium of scientific institutes with main hardware contributions from France, USA, Japan and Germany.

  19. Synchronised Aerosol Mass Spectrometer Measurements across Europe

    Science.gov (United States)

    Nemitz, Eiko

    2010-05-01

    Up to twelve Aerodyne Aerosol Mass Spectrometers (AMSs) were operated simultaneously at rural and background stations (EMEP and EUSAAR sites) across Europe. Measurements took place during three intensive periods, in collaboration between the European EUCAARI IP and the EMEP monitoring activities under the UNECE Convention for Long-Range Transboundary Air Pollution (CLRTAP) during three contrasting months (May 2008, Sep/Oct 2008, Feb/Mar 2009). These measurements were conducted, analysed and quality controlled carefully using a unified protocol, providing the largest spatial database of aerosol chemical composition measured with a unified online technique to date, and a unique snapshots of the European non-refractory submicron aerosol climatology. As campaign averages over all active monitoring sites, organics represent 28 to 43%, sulphate 18 to 25%, ammonium 13 to 15% and nitrate 15 to 36% of the resolved aerosol mass, with the highest relative nitrate contribution during the Feb/Mar campaign. The measurements demonstrate that in NW Europe (e.g. Ireland, UK, The Netherlands, Germany, Switzerland) the regional submicron aerosol tends to be neutralised and here nitrates make a major contribution to the aerosol mass. By contrast, periods with low nitrate and acidic aerosol were observed at sites in S and E Europe (e.g. Greece, Finland), presumably due to a combination of larger SO2 point sources in Easter Europe, smaller local NH3 sources and, in the case of Greece, higher temperatures. While at the more marine and remote sites (Ireland, Scotland, Finland) nitrate concentrations were dominated by episodic transport phenomena, at continental sites (Switzerland, Germany, Hungary) nitrate followed a clear diurnal cycle, reflecting the thermodynamic behaviour of ammonium nitrate. The datasets clearly shows spatially co-ordinated, large-scale pollution episodes of organics, sulphate and nitrate, the latter being most pronounced during the Feb/Mar campaign. At selected

  20. 21 Tesla Fourier Transform Ion Cyclotron Resonance Mass Spectrometer: A National Resource for Ultrahigh Resolution Mass Analysis.

    Science.gov (United States)

    Hendrickson, Christopher L; Quinn, John P; Kaiser, Nathan K; Smith, Donald F; Blakney, Greg T; Chen, Tong; Marshall, Alan G; Weisbrod, Chad R; Beu, Steven C

    2015-09-01

    We describe the design and initial performance of the first 21 tesla Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer. The 21 tesla magnet is the highest field superconducting magnet ever used for FT-ICR and features high spatial homogeneity, high temporal stability, and negligible liquid helium consumption. The instrument includes a commercial dual linear quadrupole trap front end that features high sensitivity, precise control of trapped ion number, and collisional and electron transfer dissociation. A third linear quadrupole trap offers high ion capacity and ejection efficiency, and rf quadrupole ion injection optics deliver ions to a novel dynamically harmonized ICR cell. Mass resolving power of 150,000 (m/Δm(50%)) is achieved for bovine serum albumin (66 kDa) for a 0.38 s detection period, and greater than 2,000,000 resolving power is achieved for a 12 s detection period. Externally calibrated broadband mass measurement accuracy is typically less than 150 ppb rms, with resolving power greater than 300,000 at m/z 400 for a 0.76 s detection period. Combined analysis of electron transfer and collisional dissociation spectra results in 68% sequence coverage for carbonic anhydrase. The instrument is part of the NSF High-Field FT-ICR User Facility and is available free of charge to qualified users.

  1. Comprehensive multidimensional gas chromatography coupled to low resolution quadrupole mass spectrometry for the analysis of PCDDs, PCDFs and PCBs

    Energy Technology Data Exchange (ETDEWEB)

    Costa, J.P. [Universitat de Barcelona (Spain). Facultat de Quimica, Dept. de Quimica Analitica; Korytar, P.; Boer, J. de [Netherlands Institutes for Fisheries Research, Ijmuiden (Netherlands); Leonards, P. [Instituto Quimico de Sarria, Barcelona (Spain)

    2004-09-15

    Because of the high persistency and extreme toxicity of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) and so-called dioxin-like polychlorinated biphenyls (PCBs), their trace level determination is a topic of much interest. The typical concentrations of this compounds, sub-ng/kg, makes that they have to be clearly separated from other, less toxic, congeners present in the samples and from the matrix and the use of sensitive techniques is required for the quantification. The analyses of the compounds are usually done by high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC-HRMS). Recently, alternative novel techniques have been developed which are improving the chromatographic separation, e.g. comprehensive multidimensional gas chromatography (GC x GC), for the analysis of the compounds. The aim of this work is to evaluate GC x GC coupled to a low resolution quadrupole mass spectrometer for the quantification of PCDDs, PCDFs and dioxin like PCBs.

  2. Real-Time Quantitative Analysis of H2, He, O2, and Ar by Quadrupole Ion Trap Mass Spectrometry

    Science.gov (United States)

    Ottens, Andrew K.; Harrison, W. W.; Griffin, Timothy P.; Helms, William R.; Voska, N. (Technical Monitor)

    2002-01-01

    The use of a quadrupole ion trap mass spectrometer for quantitative analysis of hydrogen and helium as well as other permanent gases is demonstrated. The customized instrument utilizes the mass selective instability mode of mass analysis as with commercial instruments; however, this instrument operates at a greater RF trapping frequency and without a buffer gas. With these differences, a useable mass range from 2 to over 50 Da is achieved, as required by NASA for monitoring the Space Shuttle during a launch countdown. The performance of the ion trap is evaluated using part-per-million concentrations of hydrogen, helium, oxygen and argon mixed into a nitrogen gas stream. Relative accuracy and precision when quantitating the four analytes were better than the NASA-required minimum of 10% error and 5% deviation, respectively. Limits of detection were below the NASA requirement of 25-ppm hydrogen and 100-ppm helium; those for oxygen and argon were slightly higher than the requirement. The instrument provided adequate performance at fast data recording rates, demonstrating the utility of an ion trap mass spectrometer as a real-time quantitative monitoring device for permanent gas analysis.

  3. Inficon Transpector MPH Mass Spectrometer Random Vibration Test Report

    Science.gov (United States)

    Santiago-Bond, Jo; Captain, Janine

    2015-01-01

    The purpose of this test report is to summarize results from the vibration testing of the INFICON Transpector MPH100M model Mass Spectrometer. It also identifies requirements satisfied, and procedures used in the test. As a payload of Resource Prospector, it is necessary to determine the survivability of the mass spectrometer to proto-qualification level random vibration. Changes in sensitivity of the mass spectrometer can be interpreted as a change in alignment of the instrument. The results of this test will be used to determine any necessary design changes as the team moves forward with flight design.

  4. Miniature Mass Spectrometer for Earth Science Research Project

    Data.gov (United States)

    National Aeronautics and Space Administration — By drastically reducing the physical footprint of a mass spectrometer to the size of a beverage can, Ceramitron could set a new performance/price standard in the...

  5. An integrated ion trap and time-of-flight mass spectrometer for chemical and photo- reaction dynamics studies.

    Science.gov (United States)

    Schowalter, Steven J; Chen, Kuang; Rellergert, Wade G; Sullivan, Scott T; Hudson, Eric R

    2012-04-01

    We demonstrate the integration of a linear quadrupole trap with a simple time-of-flight mass spectrometer with medium-mass resolution (m/Δm ∼ 50) geared towards the demands of atomic, molecular, and chemical physics experiments. By utilizing a novel radial ion extraction scheme from the linear quadrupole trap into the mass analyzer, a device with large trap capacity and high optical access is realized without sacrificing mass resolution. This provides the ability to address trapped ions with laser light and facilitates interactions with neutral background gases prior to analyzing the trapped ions. Here, we describe the construction and implementation of the device as well as present representative ToF spectra. We conclude by demonstrating the flexibility of the device with proof-of-principle experiments that include the observation of molecular-ion photodissociation and the measurement of trapped-ion chemical reaction rates. © 2012 American Institute of Physics

  6. Adduct formation in liquid chromatography-triple quadrupole mass spectrometric measurement of bryostatin 1.

    Science.gov (United States)

    Nelson, Thomas J; Sen, Abhik; Alkon, Daniel L; Sun, Miao-Kun

    2014-01-01

    Bryostatin 1, a potential anti-Alzheimer drug, is effective at subnanomolar concentrations. Measurement is complicated by the formation of low m/z degradation products and the formation of adducts with various cations, which make accurate quantitation difficult. Adduct formation caused the sample matrix or mobile phase to partition bryostatin 1 into products of different mass. Degradation of the 927 [M+Na](+) ion to a 869m/z product was strongly influenced by ionization conditions. We validated a bryostatin 1 assay in biological tissues using capillary column HPLC with nanospray ionization (NSI) in a triple-quadrupole mass spectrometer in selected reaction monitoring (SRM) mode. Adduct formation was controlled by adding 1mM acetic acid and 0.1mM sodium acetate to the HPLC buffer, maximizing the formation of the [M+Na](+) ion. Efficient removal of contaminating cholesterol from the sample during solvent extraction was also critical. The increased sensitivity provided by NSI and capillary-bore columns and the elimination of signal partitioning due to adduct formation and degradation in the ionization source enabled a detection limit of 1×10(-18)mol of bryostatin 1 and a LLOQ of 3×10(-18)mol from 1μl of sample. Bryostatin 1 at low pmol/l concentrations enabled measurement in brain and other tissues without the use of radioactive labels. Despite bryostatin 1's high molecular weight, considerable brain access was observed, with peak brain concentrations exceeding 8% of the peak blood plasma concentrations. Bryostatin 1 readily crosses the blood-brain barrier, reaching peak concentrations of 0.2nM, and specifically activates and translocates brain PKCɛ. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Ion beam properties after mass filtering with a linear radiofrequency quadrupole

    Energy Technology Data Exchange (ETDEWEB)

    Ferrer, R., E-mail: Rafael.Ferrer@fys.kuleuven.be [National Superconducting Cyclotron Laboratory, Michigan State University, East Lansing, MI 48824 (United States); Kwiatkowski, A.A.; Bollen, G.; Lincoln, D.L. [National Superconducting Cyclotron Laboratory, Michigan State University, East Lansing, MI 48824 (United States); Department of Physics and Astronomy, East Lansing, MI 48824 (United States); Morrissey, D.J.; Pang, G.K. [National Superconducting Cyclotron Laboratory, Michigan State University, East Lansing, MI 48824 (United States); Department of Chemistry, East Lansing, MI 48824 (United States); Ringle, R. [National Superconducting Cyclotron Laboratory, Michigan State University, East Lansing, MI 48824 (United States); Savory, J. [National Superconducting Cyclotron Laboratory, Michigan State University, East Lansing, MI 48824 (United States); Department of Physics and Astronomy, East Lansing, MI 48824 (United States); Schwarz, S. [National Superconducting Cyclotron Laboratory, Michigan State University, East Lansing, MI 48824 (United States)

    2014-01-21

    The properties of ion beams passing through a linear radiofrequency quadrupole mass filter were investigated with special attention to their dependence on the mass resolving power. Experimentally, an increase of the transverse emittance was observed as the mass-to-charge selectivity of the mass filter was raised. The experimental behavior was confirmed by beam transport simulations. -- Highlights: • The ion-optical properties of a Quadrupole Mass Filter (QMF) are presented. • Measured beam emittances follow a trend to larger values for smaller A/Q ratios and increasing mass resolution. • The experimental behavior was confirmed by beam transport simulations. • The use of a QMF for mass filtering comes at the cost of emittance growth of the ion beam.

  8. On the transmission function of an ion-energy and mass spectrometer

    Science.gov (United States)

    Hamers, E. A. G.; van Sark, W. G. J. H. M.; Bezemer, J.; Goedheer, W. J.; van der Weg, W. F.

    1998-01-01

    The operation of a mass spectrometer system with an electrostatic energy analyser, designed for measurements of mass-resolved ion-energy distributions, is discussed. We show how the electric fields in the different electrostatic lenses present in the system can be optimized. These lenses direct the ions entering the system into the energy filter and the quadrupole mass filter. These lenses can exhibit chromatic aberration. The conditions without chromatic aberration have been found by simulating the ion trajectories in the part of the system up to the energy filter. Also, an experimental method is presented to find these settings. We show that the energy-dependent transmission of ions through the system is mainly determined by its acceptance angle. Ionenergy spectra from an argon plasma have been measured and corrected for the transmission of the ions through the system. Published by Elsevier Science B.V.

  9. DC SQUID Spectrometers for Nuclear Quadrupole and Low-Field Nuclear Magnetic Resonance Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    TonThat, Dinh M. [Univ. of California, Berkeley, CA (United States)

    1998-04-01

    The dc Superconducting Quantum Interference Device (SQUJD) is a very sensitive detector of magnetic flux, with a typical flux noise of the order of 1 μΦ0Hz-1/2 at liquid helium temperature (Φ0=h/2e). This inherent flux sensitivity of the SQUID is used in a spectrometer for the detection of nuclear magnetic resonance (NMR.)and nuclear quadruple resonance (NQR). The processing magnetic field from the nuclear spins is coupled to the SQUID by mean of a flux transformer. The SQUID NMR spectrometer is used to measure the longitudinal relaxation time T1 of solid 129Xe at 4.2 K down to 0.1 mT.

  10. Mass spectrometers based on a cone-shaped acromatic prism

    Energy Technology Data Exchange (ETDEWEB)

    Spivak-Lavrov, I.F. [Pedagogical Inst. of Aktyubinsk (Kazakhstan)

    1995-09-01

    We have elaborated a mass spectrometer without lenses consisting of one conic achromatic prism. It has a specific mass dispersion which is equal to 67.5 mm/m per 1% change of mass. (By specific dispersion we mean linear dispersion related to the main path.) The pass of charged particles with different emittance is investigated with the help of integrating precise equations for tracks of charged particles in natural curvilinear coordinates. We have calculated the resolving power and aberration of a mass spectrometer for different beams of particles. It is evident that the mass spectrometer is particularly effective in use when we deal with rather wide ion beams having an insignificant angular divergence in the mean plane. (orig.).

  11. Rapid Analysis of Components in Coptis chinensis Franch by Ultra-Performance Liquid Chromatography with Quadrupole Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Tian, Peng-peng; Zhang, Xiao-xu; Wang, Hong-ping; Li, Pu-ling; Liu, Yu-xin; Li, Shao-jing

    2017-01-01

    Background: Coptis chinensis Franch is a traditional Chinese medical herb. Objective: In this article, ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was used to rapidly, qualitatively, and comprehensively identify the components in Coptis chinensis Franch. Materials and Methods: Chromatographic separation was achieved on an Agilent Zorbax RRHD Eclipse Plus C18 column. The mobile phase consisted of 0.1% formic acid water (A) and 0.1% formic acid acetonitrile (B) with a gradient program. Qualitative analysis was performed on an Agilent 6540 quadrupole time-of-flight mass spectrometer, which was equipped with a Dual AJS ESI source operating in negative mode. Results: A total of 30 alkaloid and non-alkaloid components of Coptis chinensis Franch were identified in only 14 min. Conclusion: This study helped to provide a basis for the quality control of Coptis chinensis Franch. SUMMARY Qualitative analysis method of chlorogenic alkaloids and non-alkaloids in Coptis chinensis Franch is developed by Ultra-performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS) method.Established UPLC-Q-TOF-MS/MS analysis method is validated with rapidness and accuracy.The developed method was successfully applied for qualitative analysis of Coptis chinensis Franch sample collected from cultivation place in China. Abbreviations used: Q-TOF-MS: quadrupole time-of-flight mass spectrometry, UPLC: ultra-performance liquid chromatography, pos: positive, neg: negative. Q-TOF-MS: quadrupole time-of-flight mass spectrometry, UPLC: ultra-performance liquid chromatography, pos: positive, neg: negative. UPLC: ultra-performance liquid chromatography, pos: positive, neg: negative. pos: positive, neg: negative. neg: negative. PMID:28216903

  12. ACTRIS ACSM intercomparison - Part I: Reproducibility of concentration and fragment results from 13 individual Quadrupole Aerosol Chemical Speciation Monitors (Q-ACSM) and consistency with Time-of-Flight ACSM (ToF-ACSM), High Resolution ToF Aerosol Mass Spectrometer (HR-ToF-AMS) and other co-located instruments

    Science.gov (United States)

    Crenn, V.; Sciare, J.; Croteau, P. L.; Verlhac, S.; Fröhlich, R.; Belis, C. A.; Aas, W.; Äijälä, M.; Alastuey, A.; Artiñano, B.; Baisnée, D.; Bonnaire, N.; Bressi, M.; Canagaratna, M.; Canonaco, F.; Carbone, C.; Cavalli, F.; Coz, E.; Cubison, M. J.; Esser-Gietl, J. K.; Green, D. C.; Gros, V.; Heikkinen, L.; Herrmann, H.; Lunder, C.; Minguillón, M. C.; Močnik, G.; O'Dowd, C. D.; Ovadnevaite, J.; Petit, J.-E.; Petralia, E.; Poulain, L.; Priestman, M.; Riffault, V.; Ripoll, A.; Sarda-Estève, R.; Slowik, J. G.; Setyan, A.; Wiedensohler, A.; Baltensperger, U.; Prévôt, A. S. H.; Jayne, J. T.; Favez, O.

    2015-07-01

    As part of the European ACTRIS project, the first large Quadrupole Aerosol Chemical Speciation Monitor (Q-ACSM) intercomparison study was conducted in the region of Paris for three weeks during the late fall-early winter period (November-December 2013). The first week was dedicated to tuning and calibration of each instrument whereas the second and third were dedicated to side-by-side comparison in ambient conditions with co-located instruments providing independent information on submicron aerosol optical, physical and chemical properties. Near real-time measurements of the major chemical species (organic matter, sulfate, nitrate, ammonium and chloride) in the non-refractory submicron aerosols (NR-PM1) were obtained here from 13 Q-ACSM. The results show that these instruments can produce highly comparable and robust measurements of the NR-PM1 total mass and its major components. Taking the median of the 13 Q-ACSM as a reference for this study, strong correlations (r2 > 0.9) were observed systematically for each individual ACSM across all chemical families except for chloride for which three ACSMs showing weak correlations partly due to the very low concentrations during the study. Reproducibility expanded uncertainties of Q-ACSM concentration measurements were determined using appropriate methodologies defined by the International Standard Organization (ISO 17025) and were found to be of 9, 15, 19, 28 and 36 % for NR-PM1, nitrate, organic matter, sulfate and ammonium respectively. However, discrepancies were observed in the relative concentrations of the constituent mass fragments for each chemical component. In particular, significant differences were observed for the organic fragment at mass-to-charge ratio 44, which is a key parameter describing the oxidation state of organic aerosol. Following this first major intercomparison exercise of a large number of ACSMs, detailed intercomparison results are presented as well as a discussion of some recommendations

  13. Triple Quadrupole Versus High Resolution Quadrupole-Time-of-Flight Mass Spectrometry for Quantitative LC-MS/MS Analysis of 25-Hydroxyvitamin D in Human Serum

    Science.gov (United States)

    Geib, Timon; Sleno, Lekha; Hall, Rabea A.; Stokes, Caroline S.; Volmer, Dietrich A.

    2016-08-01

    We describe a systematic comparison of high and low resolution LC-MS/MS assays for quantification of 25-hydroxyvitamin D3 in human serum. Identical sample preparation, chromatography separations, electrospray ionization sources, precursor ion selection, and ion activation were used; the two assays differed only in the implemented final mass analyzer stage; viz. high resolution quadrupole-quadrupole-time-of-flight (QqTOF) versus low resolution triple quadrupole instruments. The results were assessed against measured concentration levels from a routine clinical chemiluminescence immunoassay. Isobaric interferences prevented the simple use of TOF-MS spectra for extraction of accurate masses and necessitated the application of collision-induced dissociation on the QqTOF platform. The two mass spectrometry assays provided very similar analytical figures of merit, reflecting the lack of relevant isobaric interferences in the MS/MS domain, and were successfully applied to determine the levels of 25-hydroxyvitamin D for patients with chronic liver disease.

  14. Analysis of lightweight gases by quadrupole ion trap mass spectrometry for the safety of the American Space Shuttle program

    Science.gov (United States)

    Ottens, Andrew Keith

    The quadrupole ion trap mass spectrometer (QITMS) was patented nearly 50 years ago, when it was proposed for trace analysis of lightweight gas mixtures. Though a commercial success, QITMS has been used with analytes of ever-increasing size. We evaluated QITMS for quantifying lightweight gas mixtures with the performance compared to other mass analyzer technologies. The National Aeronautics and Space Administration (NASA) uses mass spectrometers to monitor the amount of hydrogen, helium, oxygen, and argon in the nitrogen-purged Space Shuttle. The explosive hazard of the cryogenic hydrogen and oxygen used to propel the Space Shuttle makes leak detection imperative. The two present-day leak detectors are remotely located because of their large size and sensitivity to vibration. Analysis is delayed by up to 45 s, and only two samples can be monitored simultaneously. In 2000, NASA initiated the Advanced Hazardous Gas Detection project to develop a compact, rugged, and fast mass spectrometer to be placed in multiple locations next to the Space Shuttle to provide real-time analysis with increased redundancy. The QITMS instrumentation was modified specifically for this application. The RF drive frequency was increased to 2.5 MHz to adequately trap lightweight hydrogen and helium ions. Internal ionization was preferred for use without a collision gas, along with an open source configuration that provided rapid sample replacement. The modern electronics incorporated were controlled by customized software. Analytes were found to react rapidly with abundant background gases. The QITMS operating conditions were optimized to minimize negative effects of ion-molecule reactions while maximizing analytical performance. A custom segmented scan function was developed with a total scan time of 14 ms, averaging 70 scans per data point at the required 1 Hz update rate. The QITMS met requirements for detection limits, accuracy, precision, response time, and recovery time. The linear

  15. First Results From the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

    Science.gov (United States)

    Niemann, Hasso B.; Demick, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Raaen, E.; Way, S.; Atreya, S.; Carignan, G.; Bauer, S.

    2005-01-01

    The Huygens Probe of the Cassini Huygens Mission entered the atmosphere of the moon Titan on January 14,2005. The GCMS was part of the instrument complement on the Probe to measure in situ the chemical composition of the atmosphere during the probe descent and to support the Aerosol Collector Pyrolyser (ACP) experiment by serving as detector for the pyrolization products. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns. The mass spectrometer employed five electron impact ion sources with available electron energies of either 70 or 25 eV. Three ion sources served as detectors for the GC columns and two were dedicated to direct atmosphere sampling and ACP gas sampling, respectively. The GCMS gas inlet was heated to prevent condensation, and served to evaporate surface constituents after impact.

  16. The use of stability bands to improve the performance of quadrupole mass filters

    Science.gov (United States)

    Sudakov, M. Yu.; Mamontov, E. V.

    2017-01-01

    The possibility of increasing the resolving power of quadrupole mass filters has been discussed. It has been shown that the limitations associated with the finite time of flight imposed by Von Zahn's rule are modified while using the islands of stability that appear when quadrupole is excited by the additional signals. By calculation of the exponential increment of growth of the oscillation amplitude the effect of the acceleration of mass separation and improvement of the peak shape, when the islands of stability are used for ion filtering, is explained. The case of the excitation by two signals at different frequencies has been studied theoretically. The conditions under which suppression of the first order resonance for one of the directions of motion is obtained. The direct modeling of the peak shape of the mass filter shows the possibility of obtaining a resolution of 10,000 with a time of flight of ions through the quadrupole of 100 cycles of the main RF supply, and low sensitivity of the new operating mode to the nonlinear field distortions in the quadrupoles with rods of circular cross sections.

  17. Direct current superconducting quantum interference device spectrometer for pulsed nuclear magnetic resonance and nuclear quadrupole resonance at frequencies up to 5 MHz

    Science.gov (United States)

    TonThat, Dinh M.; Clarke, John

    1996-08-01

    A spectrometer based on a dc superconducting quantum interference device (SQUID) has been developed for the direct detection of nuclear magnetic resonance (NMR) or nuclear quadrupole resonance (NQR) at frequencies up to 5 MHz. The sample is coupled to the input coil of the niobium-based SQUID via a nonresonant superconducting circuit. The flux locked loop involves the direct offset integration technique with additional positive feedback in which the output of the SQUID is coupled directly to a low-noise preamplifier. Precession of the nuclear quadrupole spins is induced by a magnetic field pulse with the feedback circuit disabled; subsequently, flux locked operation is restored and the SQUID amplifies the signal produced by the nuclear free induction signal. The spectrometer has been used to detect 27Al NQR signals in ruby (Al2O3[Cr3+]) at 359 and 714 kHz.

  18. Generalized Kerr spacetime with an arbitrary mass quadrupole moment: geometric properties vs particle motion

    CERN Document Server

    Bini, Donato; Luongo, Orlando; Quevedo, Hernando

    2009-01-01

    An exact solution of Einstein's field equations in empty space first found in 1985 by Quevedo and Mashhoon is analyzed in detail. This solution generalizes Kerr spacetime to include the case of matter with arbitrary mass quadrupole moment and is specified by three parameters, the mass $M$, the angular momentum per unit mass $a$ and the quadrupole parameter $q$. It reduces to the Kerr spacetime in the limiting case $q=0$ and to the Erez-Rosen spacetime when the specific angular momentum $a$ vanishes. The geometrical properties of such a solution are investigated. Causality violations, directional singularities and repulsive effects occur in the region close to the source. Geodesic motion and accelerated motion are studied on the equatorial plane which, due to the reflection symmetry property of the solution, turns out to be also a geodesic plane.

  19. Generalized Kerr spacetime with an arbitrary mass quadrupole moment: geometric properties versus particle motion

    Energy Technology Data Exchange (ETDEWEB)

    Bini, Donato [Istituto per le Applicazioni del Calcolo ' M. Picone' , CNR I-00185 Rome (Italy); Geralico, Andrea; Luongo, Orlando; Quevedo, Hernando, E-mail: binid@icra.i [ICRA, University of Rome ' La Sapienza' , I-00185 Rome (Italy)

    2009-11-21

    An exact solution of Einstein's field equations in empty space first found in 1985 by Quevedo and Mashhoon is analyzed in detail. This solution generalizes Kerr spacetime to include the case of matter with an arbitrary mass quadrupole moment and is specified by three parameters, the mass M, the angular momentum per unit mass a and the quadrupole parameter q. It reduces to the Kerr spacetime in the limiting case q = 0 and to the Erez-Rosen spacetime when the specific angular momentum a vanishes. The geometrical properties of such a solution are investigated. Causality violations, directional singularities and repulsive effects occur in the region close to the source. Geodesic motion and accelerated motion are studied on the equatorial plane which, due to the reflection symmetry property of the solution, also turns out to be a geodesic plane.

  20. Pharmaceutical metabolite profiling using quadrupole/ion mobility spectrometry/time-of-flight mass spectrometry.

    Science.gov (United States)

    Chan, Eric C Y; New, Lee Sun; Yap, Chun Wei; Goh, Lin Tang

    2009-02-01

    The use of hybrid quadrupole ion mobility spectrometry time-of-flight mass spectrometry (Q/IMS/TOFMS) in the metabolite profiling of leflunomide (LEF) and acetaminophen (APAP) is presented. The IMS drift times (T(d)) of the drugs and their metabolites were determined in the IMS/TOFMS experiments and correlated with their exact monoisotopic masses and other in silico generated structural properties, such as connolly molecular area (CMA), connolly solvent-excluded volume (CSEV), principal moments of inertia along the X, Y and Z Cartesian coordinates (MI-X, MI-Y and MI-Z), inverse mobility and collision cross-section (CCS). The correlation of T(d) with these parameters is presented and discussed. IMS/TOF tandem mass spectrometry experiments (MS(2) and MS(3)) were successfully performed on the N-acetyl-p-benzoquinoneimine glutathione (NAPQI-GSH) adduct derived from the in vitro microsomal metabolism of APAP. As comparison, similar experiments were also performed using hybrid triple quadrupole linear ion trap mass spectrometry (QTRAPMS) and quadrupole time-of-flight mass spectrometry (QTOFMS). The abilities to resolve the product ions of the metabolite within the drift tube and fragment the ion mobility resolved product ions in the transfer travelling wave-enabled stacked ring ion guide (TWIG) demonstrated the potential applicability of the Q/IMS/TOFMS technique in pharmaceutical metabolite profiling.

  1. Recent results from the Penning trap mass spectrometer ISOLTRAP

    CERN Document Server

    Blaum, Klaus; Beck, D; Bollen, Georg; Delahaye, P; Guenaut, C; Herfurth, F; Kellerbauer, Alban G; Kluge, H J; Lunney, M D; Rodríguez, D; Schwarz, S; Schweikhard, L; Weber, C; Yazidjian, C

    2004-01-01

    In the last few years a number of new scientific highlights have been obtained by ISOLTRAP, the tandem Penning trap mass spectrometer for on-line mass measurements of short-lived radionuclides. The precise determination of nuclear binding energies far from stability includes nuclei that are produced at rates of 100 ions/s and with half-lives below 100 ms. The mass resolving power reaches 10$^{7}$ and the uncertainty of the resulting mass values has been pushed down to $1 \\times 10^{-8}$. In this article recent ISOLTRAP mass measurements are summarized and the current status of ISOLTRAP is presented.

  2. Aerosol quantification with the Aerodyne Aerosol Mass Spectrometer: detection limits and ionizer background effects

    Directory of Open Access Journals (Sweden)

    S. Borrmann

    2009-02-01

    Full Text Available Systematic laboratory experiments were performed to investigate quantification of various species with two versions of the Aerodyne Aerosol Mass Spectrometer, a Quadrupole Aerosol Mass Spectrometer (Q-AMS and a compact Time-of-Flight Aerosol Mass Spectrometer (c-ToF-AMS. Here we present a new method to continuously determine the detection limits of the AMS analyzers during regular measurements, yielding detection limit (DL information under various measurement conditions. Minimum detection limits range from 0.03 μg m−3 (nitrate, sulfate, and chloride up to 0.5 μg m−3 (organics for the Q-AMS. Those of the c-ToF-AMS are found between 0.003 μg m−3 (nitrate, sulfate and 0.03 μg m−3 (ammonium, organics. The DL values found for the c-ToF-AMS were ~10 times lower than those of the Q-AMS, mainly due to differences in ion duty cycle. Effects causing an increase of the detection limits include long-term instrument contamination, measurement of high aerosol mass concentrations and short-term instrument history. The self-cleaning processes which reduce the instrument background after measurement of large aerosol concentrations as well as the influences of increased instrument background on mass concentration measurements are discussed. Finally, improvement of detection limits by extension of averaging time intervals, selected or reduced ion monitoring, and variation of particle-to-background measurement ratio are investigated.

  3. The Neutral Gas and Ion Mass Spectrometer on the Mars Atmosphere and Volatile Evolution Mission

    Science.gov (United States)

    Mahaffy, Paul R.; Benna, Mehdi; King, Todd; Harpold, Daniel N.; Arvey, Robert; Barciniak, Michael; Bendt, Mirl; Carrigan, Daniel; Errigo, Therese; Holmes, Vincent; Kellogg, James; Jaeger, Ferzan; Raaen, Eric; Tan, Florence

    2014-01-01

    The Neutral Gas and Ion Mass Spectrometer (NGIMS) of the Mars Atmosphere and Volatile Evolution Mission (MAVEN) is designed to measure the composition, structure, and variability of the upper atmosphere of Mars. The NGIMS complements two other instrument packages on the MAVEN spacecraft designed to characterize the neutral upper atmosphere and ionosphere of Mars and the solar wind input to this region of the atmosphere. The combined measurement set is designed to quantify atmosphere escape rates and provide input to models of the evolution of the martian atmosphere. The NGIMS is designed to measure both surface reactive and inert neutral species and ambient ions along the spacecraft track over the 125-500 km altitude region utilizing a dual ion source and a quadrupole analyzer.

  4. The Neutral Mass Spectrometer on the Lunar Atmosphere and Dust Environment Explorer Mission

    Science.gov (United States)

    Mahaffy, Paul R.; Hodges, R. Richard; Benna, Mehdi; King, Todd; Arvey, Robert; Barciniak, Michael; Bendt, Mirl; Carigan, Daniel; Errigo, Therese; Harpold, Daniel N.; Holmes, Vincent; Johnson, Christopher S.; Kellogg, James; Kimvilakani, Patrick; Lefavor, Matthew; Hengemihle, Jerome; Jaeger, Ferzan; Lyness, Eric; Maurer, John; Nguyen, Daniel; Nolan, Thomas; Noreiga, Felix; Noreiga, Marvin; Patel, Kiran; Prats, Benito; Quinones, Omar; Raaen, Eric; Tan, Florence; Weidner, Edwin; Woronowicz, Michael; Gundersen, Cynthia (Inventor); Battel, Steven; Block, Bruce P.; Arnett, Ken; Miller, Ryan

    2014-01-01

    The Neutral Mass Spectrometer (NMS) of the Lunar Atmosphere and Dust Environment Explorer (LADEE) Mission is designed to measure the composition and variability of the tenuous lunar atmosphere. The NMS complements two other instruments on the LADEE spacecraft designed to secure spectroscopic measurements of lunar composition and in situ measurement of lunar dust over the course of a 100-day mission in order to sample multiple lunation periods. The NMS utilizes a dual ion source designed to measure both surface reactive and inert species and a quadrupole analyzer. The NMS is expected to secure time resolved measurements of helium and argon and determine abundance or upper limits for many other species either sputtered or thermally evolved from the lunar surface.

  5. A mass spectrometer for pain-response monitoring in rats

    Science.gov (United States)

    Elizarov, A. Yu.

    2017-06-01

    A mass spectrometer with a membrane interface has been used for measuring the relative concentration of carbon dioxide (CO2) released from rat skin in response to thermal irritation and pain stimulus during intraperitoneal propofol-lidocaine anesthesia. It is established that the local anesthetic lidocaine directly influences the central nervous system and induces antinociceptive reaction to thermal irritation.

  6. Injection system of the minicyclotron accelerator mass spectrometer

    Institute of Scientific and Technical Information of China (English)

    LIUYonghao; LIDeming; 等

    1999-01-01

    The existing injection system of the SMCAMS(super-sensitive minicyclotron accelerator mass spectrometer)is described together with the discussion of its disadvantages exposed after having been operating for five years.which provides a basis for consideration of improvements to the injection system.An optimized injection system with an analytical magent added prior to the minicryclotron has been proposed and calculated.

  7. Ion Mass Spectrometer Development for JEO Class Missions

    Science.gov (United States)

    Sittler, E. C.; Cooper, J. F.; Paschalidis, N.; Coplan, M. A.; Chornay, D. J.; Sturner, S. J.; Brown, S. K.; Hartle, R. E.; Paterson, W. R.

    2012-10-01

    Under the Astrobiology Instrument Development Program we have been developing an advanced 3-D ion mass spectrometer (IMS) from 10 V to 30 kV, that can be proposed for missions to Jupiter's icy moons, Uranus, Titan, asteroids, comets, and solar wind.

  8. Quantification of sterol lipids in plants by quadrupole time-of-flight mass spectrometry

    OpenAIRE

    Wewer, Vera; Dombrink, Isabel; vom Dorp, Katharina; Dörmann, Peter

    2011-01-01

    Glycerolipids, sphingolipids, and sterol lipids constitute the major lipid classes in plants. Sterol lipids are composed of free and conjugated sterols, i.e., sterol esters, sterol glycosides, and acylated sterol glycosides. Sterol lipids play crucial roles during adaption to abiotic stresses and plant-pathogen interactions. Presently, no comprehensive method for sterol lipid quantification in plants is available. We used nanospray ionization quadrupole-time-of-flight mass spectrometry (Q-TOF...

  9. Series fabrication of the main quadrupole cold masses for the LHC begins

    CERN Multimedia

    2003-01-01

    Three hundred and sixty main quadrupole (MQ) magnets will perform the principal beam focusing around the 27 km LHC ring. CERN and CEA-Saclay began collaborating on the development and prototyping of these magnets in 1989. This resulted in five highly successful quadrupole units - also known as short straight sections - one of which was integrated for testing in String 1, and two others of the final design in String 2. Once the tests had confirmed the validity of the design and realization, the fabrication of the 360 cold masses had to be transferred to industry.The German firm ACCEL Instruments was entrusted both with the construction of the quadrupole magnets themselves, and with their assembly into the cold masses together with various combinations of corrector magnets produced by other European manufacturers. Here we see the first of the cold masses containing the MQ magnet of the machine arcs together with two types of corrector magnet ready for shipping to CERN. Pictured with this first unit, delivered o...

  10. Series fabrication of the main quadrupole cold masses for the LHC begins

    CERN Multimedia

    2003-01-01

    Three hundred and sixty main quadrupole (MQ) magnets will perform the principal beam focusing around the 27 km LHC ring. CERN and CEA-Saclay began collaborating on the development and prototyping of these magnets in 1989. This resulted in five highly successful quadrupole units - also known as short straight sections - one of which was integrated for testing in String 1, and two others of the final design in String 2. Once the tests had confirmed the validity of the design and realization, the fabrication of the 360 cold masses had to be transferred to industry.The German firm ACCEL Instruments was entrusted both with the construction of the quadrupole magnets themselves, and with their assembly into the cold masses together with various combinations of corrector magnets produced by other European manufacturers. Here we see the first of the cold masses containing the MQ magnet of the machine arcs together with two types of corrector magnet ready for shipping to CERN. This first unit was delivered on 12 Februa...

  11. Targeted comparative proteomics by liquid chromatography/matrix-assisted laser desorption/ionization triple-quadrupole mass spectrometry.

    Science.gov (United States)

    Melanson, Jeremy E; Chisholm, Kenneth A; Pinto, Devanand M

    2006-01-01

    Here we report the first application of a matrix-assisted laser desorption/ionization (MALDI) triple-quadrupole mass spectrometer for targeted proteomics. Employing an amine-specific isotopic labelling approach, the technique was validated using five randomly selected bovine serum albumin peptides differentially labelled at known ratios. An indirect benefit of the isotopic labelling technique is a significant enhancement of the a1 ion in tandem mass (MS/MS) spectra of all peptides studied. Therefore, the a1 ion was selected as the fragment ion for multiple reaction monitoring (MRM) in all cases, eliminating tedious method development and optimization. Accurate quantification was achieved with an average relative standard deviation (RSD) of 5% (n = 5) and a detection limit of 14 amol. The technique was then applied to validate an important virulence biomarker of the fungal pathogen Candida albicans, which was not accurately quantified using global proteomics experiment employing two-dimensional liquid chromatography/electrospray ionization tandem mass spectrometry (2D-LC/ESI)-MS/MS. Using LC/MALDI-MRM analysis of five tryptic peptides, the protein PHR1 was found to be upregulated in the hyphal (pathogenic) form of C. albicans by a factor of 7.7 +/- 0.8.

  12. Comprehensive two-dimensional gas chromatography in combination with rapid scanning quadrupole mass spectrometry in perfume analysis.

    Science.gov (United States)

    Mondello, Luigi; Casillia, Alessandro; Tranchida, Peter Quinto; Dugo, Giovanni; Dugo, Paola

    2005-03-04

    Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI).

  13. The PNL high-transmission three-stage mass spectrometer

    Science.gov (United States)

    Stoffels, J. J.; Ells, D. R.; Bond, L. A.; Freedman, P. A.; Tattersall, B. N.; Lagergren, C. R.

    1992-12-01

    We have constructed a three-stage isotope-ratio mass spectrometer of unique ion-optical design that achieves high ion transmission efficiency and high abundance sensitivity. The spectrometer has tandem 90 deg deflection magnets with boundaries 18 deg off normal. The magnet drift lengths are 1.48 times the 27-cm radius of deflection. This extended geometry gives a mass dispersion equivalent to a 40-cm-radius magnet with normal boundaries. The first magnet renders the ion beam parallel in the vertical plane and provides a focus in the horizontal plane of mass dispersion. The second magnet brings the beam to a stigmatic focus. This novel ion-optical design gives 100 percent transmission without the need for intermediate focusing lenses. It also provides a 16 percent increase in mass resolution over the traditional tandem geometry with normal magnet boundaries. Complete transmission of ions is maintained through a third-stage cylindrical electric sector of 38-cm radius, which provides increased isotope-abundance sensitivity. The isotope-abundance sensitivity of the new mass spectrometer is an order of magnitude better than similar instruments with normal magnet boundaries. This is because the vertical focusing of the ion beam prevents ion scattering from the top and bottom of the flight tube. The measured values of the isotope-abundance sensitivity one-half mass unit away from the rhenium ion peaks at masses 185 and 187 are M - 1/2 = (6.5 +/- 0.5)(10)(exp -10) and M + 1/2 = (3.1 +/- 0.8)(10)(exp -10). By extrapolation, the uranium isotope-abundance sensitivity is M - 1 = 1(10)(exp -10). Construction of the instrument was facilitated by using standard commercial mass spectrometer components.

  14. Initial measurements with the SUERC accelerator mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, Stewart E-mail: toodeep@suerc.gla.ac.uk; Xu, Sheng; Schnabel, Christoph; Dougans, Andrew; Tait, Andrew; Kitchen, Richard; Klody, George; Loger, Roger; Pollock, Tom; Schroeder, James; Sundquist, Mark

    2004-08-01

    {sup 10}Be, {sup 14}C, {sup 36}Cl and {sup 129}I test measurements have been made with a new Pelletron-based accelerator mass spectrometer operating at up to 5.2 MV. All ion detection was with a versatile gas ionization detector. Low-background radiocarbon measurements with 2% scatter of identical samples was performed with both spectrometer ion sources. {sup 10}Be/Be backgrounds of 3 x 10{sup -15} were achieved using a gas cell adjoining the detector for {sup 10}B suppression. High sample-throughput Cl AMS with {sup 36}Cl/Cl backgrounds of 4 x 10{sup -15} was accomplished.

  15. Direct Chemical Analysis of Solids by Laser Ablation in an Ion-Storage Time-of-Flight Mass Spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Klunder, G L; Grant, P M; Andresen, B D; Russo, R E

    2003-09-29

    A laser ablation/ionization mass spectrometer system is described for the direct analysis of solids, particles, and fibers. The system uses a quadrupole ion trap operated in an ion-storage (IS) mode, coupled with a reflectron time-of-flight mass spectrometer (TOF-MS). The sample is inserted radially into the ring electrode and an imaging system allows direct viewing and selected analysis of the sample. Measurements identified trace contaminants of Ag, Sn, and Sb in a Pb target with single laser-shot experiments. Resolution (m/{micro}m) of 1500 and detection limits of approximately 10 pg have been achieved with a single laser pulse. The system configuration and related operating principles for accurately measuring low concentrations of isotopes are described.

  16. Coupling of the recoil mass spectrometer CAMEL to the {gamma}-ray spectrometer GASP

    Energy Technology Data Exchange (ETDEWEB)

    Spolaore, P. [Istituto Nazionale di Fisica Nucleare, Legnaro (Italy). Lab. Nazionali di Legnaro; Ackermann, D. [Istituto Nazionale di Fisica Nucleare, Legnaro (Italy). Lab. Nazionali di Legnaro; Bednarczyk, P. [Istituto Nazionale di Fisica Nucleare, Legnaro (Italy). Lab. Nazionali di Legnaro; De Angelis, G. [Istituto Nazionale di Fisica Nucleare, Legnaro (Italy). Lab. Nazionali di Legnaro; Napoli, D. [Istituto Nazionale di Fisica Nucleare, Legnaro (Italy). Lab. Nazionali di Legnaro; Rossi Alvarez, C. [INFN, Sezione di Padova, Padova (Italy); Bazzacco, D. [INFN, Sezione di Padova, Padova (Italy); Burch, R. [INFN, Sezione di Padova, Padova (Italy); Mueller, L. [INFN, Sezione di Padova, Padova (Italy); Segato, G.F. [Dipartimento di Fisica, Universita di Padova, Padova (Italy); Scarlassara, F. [Dipartimento di Fisica, Universita di Padova, Padova (Italy)

    1995-05-15

    A project has been realized to link the CAMEL recoil mass spectrometer to the GASP {gamma}-spectrometer in order to perform high resolution and efficiency {gamma}-recoil coincidence measurements. To preserve high flexibility and autonomy in the operation of the two complex apparatus a rough factor two of reduction in the overall heavy ion transmission was accepted in designing the optics of the particle transport from the GASP center to the CAMEL focal plane. The coupled configuration has been tested with the fusion reaction {sup 58}Ni (E=212 MeV)+{sup 64}Ni, obtaining a mass resolution of 1/300 and efficiency between similar 11% and similar 15% for different evaporation products. (orig.).

  17. Micro mass spectrometer on a chip.

    Energy Technology Data Exchange (ETDEWEB)

    Cruz, Dolores Y.; Blain, Matthew Glenn; Fleming, James Grant

    2005-11-01

    The design, simulation, fabrication, packaging, electrical characterization and testing analysis of a microfabricated a cylindrical ion trap ({mu}CIT) array is presented. Several versions of microfabricated cylindrical ion traps were designed and fabricated. The final design of the individual trap array element consisted of two end cap electrodes, one ring electrode, and a detector plate, fabricated in seven tungsten metal layers by molding tungsten around silicon dioxide (SiO{sub 2}) features. Each layer of tungsten is then polished back in damascene fashion. The SiO{sub 2} was removed using a standard release processes to realize a free-hung structure. Five different sized traps were fabricated with inner radii of 1, 1.5, 2, 5 and 10 {micro}m and heights ranging from 3-24 {micro}m. Simulations examined the effects of ion and neutral temperature, the pressure and nature of cooling gas, ion mass, trap voltage and frequency, space-charge, fabrication defects, and other parameters on the ability of micrometer-sized traps to store ions. The electrical characteristics of the ion trap arrays were determined. The capacitance was 2-500 pF for the various sized traps and arrays. The resistance was in the order of 1-2 {Omega}. The inductance of the arrays was calculated to be 10-1500 pH, depending on the trap and array sizes. The ion traps' field emission characteristics were assessed. It was determined that the traps could be operated up to 125 V while maintaining field emission currents below 1 x 10{sup -15} A. The testing focused on using the 5-{micro}m CITs to trap toluene (C{sub 7}H{sub 8}). Ion ejection from the traps was induced by termination of the RF voltage applied to the ring electrode and current measured on the collector electrode suggested trapping of ions in 1-10% of the traps. Improvements to the to the design of the traps were defined to minimize voltage drop to the substrate, thereby increasing trapping voltage applied to the ring electrode, and to

  18. Cassini-Huygens Ion Neutral Mass Spectrometer and the Future

    Science.gov (United States)

    Waite, J. Hunter

    2014-05-01

    The Cassini-Huygens Ion Neutral Mass Spectrometer (Cassini INMS) designed and built by Hasso Niemann has revolutionized our understanding of the Saturn system and demonstrated the importance of mass spectrometry as a tool for understanding formation, evolution, and chemical processes. In this talk that honors the accomplishments of Hasso I will discuss: 1) the major discoveries of INMS at Titan, Enceladus, and the other icy moons of Saturn, 2) the new perspective this has given us on understanding the formation and evolution of the outer solar system, and 3) the implications for future studies in the outer solar system using mass spectrometry.

  19. Software development for a fluid portable ion trap mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Hart, K.J.; Buchanan, M.V.; Wise, M.B. [Oak Ridge National Lab., TN (United States)

    1994-12-31

    Most mass spectrometer data systems are developed and optimized for the benchtop GC/MS market and thus do not adequately address the requirements for direct sampling methods. Field analysis also places greater demands on real-time data processing including automated interpretation and quantification for target analytes. The current field portable ion trap mass spectrometers developed at ORNL are based on the Finnigan Magnum ion trap mass spectrometer which provides a procedure language for user programs. A series of these procedures has been developed to support direct sampling ion trap mass spectrometry studies and is part of an overall software development strategy to address the needs of these direct sampling instruments for rapid field analysis and process monitoring. The general approach has been to create task oriented menus that lead a user through a complete analysis. Thus, the user is focused on completing tasks rather than learning and using all of the software components to complete the task. Additionally, user input has been minimized to save keyboard input and data logging time.

  20. An improved method for the determination of 5-hydroxymethylfurfural in Shenfu injection by direct analysis in real time-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Gao, Wen; Qi, Lian-Wen; Liu, Charles C; Wang, Rui; Li, Ping; Yang, Hua

    2016-07-01

    The emergence of direct analysis in real time (DART) ion source provides the great possibility for rapid analysis of hazardous substance in drugs. DART mass spectrometry (DART-MS) enabled the conducting of a fast and non-contact analysis of various samples, including solid or liquid ones, without complex sample preparation or chromatographic separation. In this study, a modified DART-quadrupole time-of-flight mass spectrometry (DART-QTOF-MS) method was developed for identification and determination of 5-hydroxymethylfurfural (5-HMF) in Shenfu (SF) injection. The quantitative transfer of sample solution was introduced to the glass tips of DIP-it sampler at a fixed volume, which significantly increases the repeatability and accuracy of analytical results. The protonated ion of dibutyl phthalate in the atmosphere was used as the reference mass for TOF-MS recalibration during the data acquisition for constant high accuracy mass measurements. Finally, the developed DART-MS method was used to determine 5-HMF in seven batches of SF injection, and the contents of 5-HMF were not higher than 100 µg/mL. The results obtained were further confirmed by an ultra-high performance liquid chromatography combined with triple quadrupole mass spectrometer (UHPLC-QQQ-MS). The overall results demonstrated that the DART-QTOF-MS method could be applied as an alternative technique for rapid monitoring 5-HMF in herbal medicine injection. Copyright © 2015 John Wiley & Sons, Ltd.

  1. Multiple gas analyses using a mobile mass spectrometer

    Science.gov (United States)

    McCarthy, J.H.; Bigelow, R.C.

    1990-01-01

    A truck-mounted mass-spectrometer gas analyzer is described and field examples of its use are given. This unit provides a gas analyzer that can be used in the field to rapidly analyze a large number of gases. It has enabled us to establish that gas anomalies occur over a variety of deposit types and in different environments. Gases may prove to be useful geochemical indicators in exploration for concealed mineral deposits. ?? 1990.

  2. MEMS ion source for mass spectrometer integrated on a chip

    Science.gov (United States)

    Szyszka, P.; Grzebyk, T.; Górecka-Drzazga, A.; Dziuban, J. A.

    2016-11-01

    The paper describes silicon-glass MEMS electron impact ion source developed for miniature mass spectrometer (MS) integrated on a chip. The device consists of the field emission electron source with an electrophoretically deposited carbon nanotube cathode and ion beam formation electrodes. Ion source structure has been fabricated using MEMS technology. A complete manufacturing process of the test structures has been successfully elaborated and implemented.

  3. Study of quadrupole collectivity in odd mass Po and Bi isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Pai, H.; Reese, M.; Pietralla, N. [Institut fuer Kernphysik, Technische Universitaet Darmstadt, D-64289 Darmstadt (Germany); Cortes, M.L. [Institut fuer Kernphysik, Technische Universitaet Darmstadt, D-64289 Darmstadt (Germany); GSI Helmholtzzentrum fuer Schwerionenforschung GmbH, D-64291 Darmstadt (Germany); Gerl, J.; Gorska, M. [GSI Helmholtzzentrum fuer Schwerionenforschung GmbH, D-64291 Darmstadt (Germany); Podolyak, Zs. [Department of Physics, University of Surrey, Guildford, GU2 7XH (United Kingdom); Rudolph, D. [Department of Physics, Lund University, SE-22100 Lund (Sweden); Collaboration: S429 PreSPEC-AGATA-Collaboration

    2015-07-01

    Relativistic Coulomb excitations of odd-mass Po and Bi isotopes were performed during the PreSPEC-AGATA campaign at GSI to study the quadrupole collectivity in the direct vicinity of the heaviest stable doubly-magic nucleus {sup 208}Pb. The PreSPEC-AGATA campaign is the predecessor of the HISPEC (High-resolution In-flight Spectroscopy) experiment in the FAIR context. It was running 2012 and 2014 at GSI. Up to 23 AGATA crystals were used in this campaign, located behind the FRagment Separator. We present the status of the ongoing data analysis and discuss the challenges of data analysis for this type of experiments.

  4. A new method for quantifying N-nitrosamines in wastewater samples by gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Yoon, Suchul; Nakada, Norihide; Tanaka, Hiroaki

    2012-08-15

    We developed a methodology for the separation, identification, and quantification of eight N-nitrosamines. For a range of wastewater samples, including raw sewage and final-discharge wastewater, the methodology, which was based on solid-phase extraction (SPE) and a purification technique followed by analysis using a gas chromatograph equipped with a triple-quadrupole mass spectrometer, gave effective separation of the targeted compounds. The limits of detection of this method for N-nitrosamines in wastewaters ranged from 0.1 to 1.0 ng L(-1) and the limits of quantification ranged from 0.4 to 3.3 ng L(-1). As a result of preliminary recovery testing, we decided on a combination of two types of sorbent cartridges for SPE-one was aminoprophyl for sample purification and the other was activated charcoal for analyte concentration-that gave excellent recovery rates (98% to 152%) of three deuterided nitrosamines (surrogates). Using this combination of SPE, internal surrogates, and an injection surrogate, we obtained good recovery rates (80% to 131%) with low relative standard deviations (1% to 14%, n=3) for eight N-nitrosamines in all samples of influent, secondary effluent, and final discharge. We applied the newly developed pre-treatment method to an influent wastewater samples. All of the N-nitrosamines except two (NMEA and NDPA) were detected in the influent sample, at 1 to 1057 ng L(-1).

  5. Characterization of goat colostrum oligosaccharides by nano-liquid chromatography on chip quadrupole time-of-flight mass spectrometry and hydrophilic interaction liquid chromatography-quadrupole mass spectrometry.

    Science.gov (United States)

    Martín-Ortiz, A; Salcedo, J; Barile, D; Bunyatratchata, A; Moreno, F J; Martin-García, I; Clemente, A; Sanz, M L; Ruiz-Matute, A I

    2016-01-08

    A detailed qualitative and quantitative characterization of goat colostrum oligosaccharides (GCO) has been carried out for the first time. Defatted and deproteinized colostrum samples, previously treated by size exclusion chromatography (SEC) to remove lactose, were analyzed by nanoflow liquid chromatography-quadrupole-time of flight mass spectrometry (Nano-LC-Chip-Q-TOF MS). Up to 78 oligosaccharides containing hexose, hexosamine, fucose, N-acetylneuraminic acid or N-glycolylneuraminic acid monomeric units were identified in the samples, some of them detected for the first time in goat colostra. As a second step, a hydrophilic interaction liquid chromatography coupled to mass spectrometry (HILIC-MS) methodology was developed for the separation and quantitation of the main GCO, both acidic and neutral carbohydrates. Among other experimental chromatographic conditions, mobile phase additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry of target carbohydrates. Narrow peaks (wh: 0.2-0.6min) and good symmetry (As: 0.8-1.4) were obtained for GCO using an acetonitrile:water gradient with 0.1% ammonium hydroxide at 40°C. These conditions were selected to quantify the main oligosaccharides in goat colostrum samples. Values ranging from 140 to 315mgL(-1) for neutral oligosaccharides and from 83 to 251mgL(-1) for acidic oligosaccharides were found. The combination of both techniques resulted to be useful to achieve a comprehensive characterization of GCO.

  6. Liquid chromatography tandem mass spectrometric quantitation of sulfamethazine and its metabolites: direct analysis of swine urine by triple quadrupole and by ion trap mass spectrometry.

    Science.gov (United States)

    Bartolucci, G; Pieraccini, G; Villanelli, F; Moneti, G; Triolo, A

    2000-01-01

    This work describes a new method for the quantitation of trace amounts of sulfamethazine (SMZ) and its main metabolite, N4-acetylsulfamethazine (Ac-SMZ), in swine urine, using high-performance liquid chromatography (HPLC) tandem mass spectrometric analysis of crude urine after addition of internal standard and simple dilution with water. The aim was to determine whether residues of this sulfamidic drug, normally administered to swine in order to prevent infectious diseases, were present in urine at levels lower than those permitted by regulatory authorities before human consumption (EU Project SMT, contract number CT 96-2092). A 10 microL volume of diluted urine was injected into a very short, narrow-bore chromatographic column (Zorbax SB-C18 2.1 i. d. x30 mm length, 3.5 microm pore size). Elution of the analytes of interest was achieved in less than seven minutes using a rapid gradient (from 20 to 80% methanol in 3 minutes). Either a PE Sciex API 365 triple quadrupole (QqQ), operated in the selected reaction monitoring (SRM) mode, or a Finnigan LCQ ion trap (IT) mass spectrometer, operated in narrow-range product ion scan, was used as the final detector. Electrospray (ESI) was used as the ionization technique. A comparison of the two tandem mass spectrometers was performed by analyzing the same set of test samples, at three concentration levels, on three different days. Linearity of responses of the calibration standards, intra- and inter-assay precision of the samples, specificity and limits of detection were evaluated for both systems. Both the QqQ and the IT instrument was suitable for rapid, sensitive and specific determination of the analytes, although the overall performance of the QqQ was slightly superior in terms of linearity, precision and sensitivity.

  7. Ion trap with integrated time-of-flight mass spectrometer

    CERN Document Server

    Schneider, Christian; Yu, Peter; Hudson, Eric R

    2015-01-01

    Recently, we reported an ion trap experiment with an integrated time-of-flight mass spectrometer (TOFMS) [Phys. Rev. Appl. 2, 034013 (2014)] focussing on the improvement of mass resolution and detection limit due to sample preparation at millikelvin temperatures. The system utilizes a radio-frequency (RF) ion trap with asymmetric drive for storing and manipulating laser-cooled ions and features radial extraction into a compact $275$ mm long TOF drift tube. The mass resolution exceeds $m / \\Delta m = 500$, which provides isotopic resolution over the whole mass range of interest in current experiments and constitutes an improvement of almost an order of magnitude over other implementations. In this manuscript, we discuss the experimental implementation in detail, which is comprised of newly developed drive electronics for generating the required voltages to operate RF trap and TOFMS, as well as control electronics for regulating RF outputs and synchronizing the TOFMS extraction.

  8. Proton Transfer Time-of-Flight Mass Spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Watson, Thomas B [Brookhaven National Lab. (BNL), Upton, NY (United States)

    2016-03-01

    The Proton Transfer Reaction Mass Spectrometer (PTRMS) measures gas-phase compounds in ambient air and headspace samples before using chemical ionization to produce positively charged molecules, which are detected with a time-of-flight (TOF) mass spectrometer. This ionization method uses a gentle proton transfer reaction method between the molecule of interest and protonated water, or hydronium ion (H3O+), to produce limited fragmentation of the parent molecule. The ions produced are primarily positively charged with the mass of the parent ion, plus an additional proton. Ion concentration is determined by adding the number of ions counted at the molecular ion’s mass-to-charge ratio to the number of air molecules in the reaction chamber, which can be identified according to the pressure levels in the reaction chamber. The PTRMS allows many volatile organic compounds in ambient air to be detected at levels from 10–100 parts per trillion by volume (pptv). The response time is 1 to 10 seconds.

  9. A rapid method for chemical fingerprint analysis of Pan Panax notoginseng powders by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Liu, Peng; Yu, He-Shuil; Zhang, Li-Juan; Song, Xin-Bo; Kang, Li-Ping; Liu, Jing-Yuan; Zhang, Jie; Cao, Man; Yu, Kate; Kang, Ting-Guo; Ma, Bai-Ping

    2015-06-01

    A method coupling ultra-performance liquid chromatography (UPLC) with quadrupole time-of-flight mass spectrometer (Qtof MS) using the electrospray ionization (ESI) source was developed for the identification of the major saponins from Panax notoginseng powder (PNP). Ten different PNP samples were analyzed and evaluated for their quality by similarity evaluation and principle component analysis (PCA). Based on the accurate mass, summarized characteristic fragmentation behaviors, retention times of different types of saponins, related botanical biogenesis, and reported chromatographic behavior of saponins, fifty-one common peaks were effectively separated and identified, including 28 protopanaxadiol saponins and 18 protopanaxatriol saponins. Simultaneously, 15 significant discrepancy compounds were identified from the disqualified PNP samples. The established UPLC/Qtof MS fingerprint method was successfully applied for profiling and identifying the major saponins of PNP, providing a fast quality evaluation tool for distinguishing the authentic PNP and the adulterated products.

  10. Comparison of quadrupole and ion trap mass spectrometry for the analysis of polychlorinated biphenyls

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, E.; DeVita, W. [Univ. of Wisconsin, Stevens Point, WI (United States)

    1995-12-31

    Polychlorinated biphenyls (PCBs) are often analyzed using gas chromatography with an electron capture detector (GC/ECD) because of the sensitivity of this detection technique toward this class of compounds. However, use of gas chromatography/mass spectrometry (GC/MS) can provide additional selectivity, thus minimizing the likelihood of false positive results from interfering compounds. GC/MS provides a higher degree of confidence in the identification of the chromatographic peaks, but is often limited, in comparison to GC/ECL, by its sensitivity. The two most common mass analyzers used are quadrupole and ion trap detectors. In this study the authors propose to document the capabilities of both quadrupole and ion trap analyzer for analysis of PCBs. They will compare and contrast the sensitivities and linear ranges for these compounds. Sensitivities will be assessed by signal-to-noise ratio comparisons. Linearity of the calibrated range will also be investigated through evaluation of the relative response factors versus concentration of PCB for a fixed concentration of internal standard. Estimations will be made of the appropriate linear ranges on the two instruments and comparisons made in both the full scan and selected ion modes.

  11. Titan's Topside Ionospheric Composition: Cassini Plasma Spectrometer Ion Mass Spectrometer Measurements

    Science.gov (United States)

    Sittler, Edward; Hartle, Richard; Ali, Ashraf; Cooper, John; Lipatov, Alexander; Simpson, David; Sarantos, Menelaos; Chornay, Dennis; Smith, Todd

    2017-01-01

    We present ion composition measurements of Titan's topside ionosphere using both T9 and T15 Cassini Plasma Spectrometer (CAPS) Ion Mass Spectrometer (IMS) measurements. The IMS is able to make measurements of Titan's ionosphere due to ionospheric outflows as originally reported for the T9 flyby. This allows one to take advantage of the unique capabilities of the CAPS IMS which measures both the mass-per-charge (M/Q) of the ions and the fragments of the ions produced inside the sensor such as carbon, nitrogen and oxygen fragments. Specific attention will be given to such ions as NH4 +, N +, O +, CH4 +, CxHy +, and HCNH + ions as examples. The CAPS IMS uses a time-of-flight (TOF) technique which accelerates ions up to 14.6 kV, so they can pass through ultra-thin carbon foils. Neutral fragments are used to measure the ion M/Q and positive fragments to measure the atomic components. We preliminarily find, by using IMS measurements of T9 and T15 ionospheric outflows, evidence for methane group ions, nitrogen ions, ammonium ions, water group ions and CnHm + ions with n = 2, 3, and 4 within Titan's topside ionosphere. E.C. Sittler acknowledges support at Goddard Space Flight Center by the CAPS Cassini Project from JPL funds under contract # NAS703001TONMO711123/1405851.

  12. Linear electric field time-of-flight ion mass spectrometer

    Science.gov (United States)

    Funsten, Herbert O.; Feldman, William C.

    2008-06-10

    A linear electric field ion mass spectrometer having an evacuated enclosure with means for generating a linear electric field located in the evacuated enclosure and means for injecting a sample material into the linear electric field. A source of pulsed ionizing radiation injects ionizing radiation into the linear electric field to ionize atoms or molecules of the sample material, and timing means determine the time elapsed between ionization of atoms or molecules and arrival of an ion out of the ionized atoms or molecules at a predetermined position.

  13. Microprocessor-Controlled Pulsed NQR Spectrometer for Automatic Acquisition of Zeeman Perturbed Nuclear Quadrupole Spin Echo Envelope Modulations (ZSEEM )

    Science.gov (United States)

    Reddy, Narsimha; Bhavsar, Arun; Narasimhan, P. T.

    1986-02-01

    A simple microprocessor-controlled pulsed NQR spectrometer system has been developed with the capability to acquire Zeeman perturbed spin echo envelope modulations (ZSEEM). The CPU of the system is based on the Intel Corporation 8085 A microprocessor. The performance of the spectrometer is illustrated with the presentation of ZSEEM spectra of NaClO3 and KClO3.

  14. Toxin screening in phytoplankton: detection and quantitation using MALDI triple quadrupole mass spectrometry.

    Science.gov (United States)

    Sleno, Lekha; Volmer, Dietrich A

    2005-03-01

    The investigation of a MALDI triple quadrupole instrument for the analysis of spirolide toxins in phytoplankton samples is described in this study. A high-frequency (kHz) laser was employed for MALDI, generating a semicontinuous ion beam, thus taking advantage of the high duty cycle obtained in sensitive triple quadrupole MRM experiments. Initially, several experimental parameters such as type of organic matrix and concentration, solvent composition, and matrix-to-analyte ratio were optimized, and their impact on sensitivity and precision of the obtained ion currents for a reference spirolide, 13-desmethyl-C, was studied. In all quantitative experiments, excellent linearities in the concentration range between 0.01 and 1.75 microg/mL were obtained, with R2 values of 0.99 or higher. The average precision of the quantitative MALDI measurements was 7.4+/-2.4% RSD. No systematic errors were apparent with this method as shown by a direct comparison to an electrospray LC/MS/MS method. Most importantly, the MALDI technique was very fast; each sample spot was analyzed in less than 5 s as compared to several minutes with the electrospray assay. To demonstrate the potential of the MALDI triple quadrupole method, its application to quantitative analysis in several different phytoplankton samples was investigated, including crude extracts and samples from mass-triggered fractionation experiments. 13-Desmethyl spirolide C was successfully quantified in these complex samples at concentration levels from 0.05 to 90.4 microg/mL (prior to dilution to have samples fall within the dynamic range of the method) without extensive sample preparation steps. The versatility of the MALDI triple quadrupole method was also exhibited for the identification of unknown spirolide analogues. Through the use of dedicated linked scan functions such as precursor ion and neutral loss scans, several spirolide compounds were tentatively identified directly from the crude extract, without the usual time

  15. Optimizing sequence coverage for a moderate mass protein in nano-electrospray ionization quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Matsuda, Ryan; Kolli, Venkata; Woods, Megan; Dodds, Eric D; Hage, David S

    2016-09-15

    Sample pretreatment was optimized to obtain high sequence coverage for human serum albumin (HSA, 66.5 kDa) when using nano-electrospray ionization quadrupole time-of-flight mass spectrometry (nESI-Q-TOF-MS). Use of the final method with trypsin, Lys-C, and Glu-C digests gave a combined coverage of 98.8%. The addition of peptide fractionation resulted in 99.7% coverage. These results were comparable to those obtained previously with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). The sample pretreatment/nESI-Q-TOF-MS method was also used with collision-induced dissociation to analyze HSA digests and to identify peptides that could be employed as internal mass calibrants in future studies of modifications to HSA.

  16. A hand-portable digital linear ion trap mass spectrometer.

    Science.gov (United States)

    Xue, Bing; Sun, Lulu; Huang, Zhengxu; Gao, Wei; Fan, Rongrong; Cheng, Ping; Ding, Li; Ma, Li; Zhou, Zhen

    2016-10-07

    A hand-portable digital linear ion trap mass spectrometer (DLIT-MS) has been developed for VOC analysis. It has a weight of 18 kg with dimensions of 49 cm × 39 cm × 16 cm, and consumes an average power of ca. 60 W. As a result of the introduction of a digital waveform, the DLIT-MS can be driven at a lower voltage (±100 V) to cover a mass range of 30-300 Th with a unit resolution. Compact electronics has been designed to control the DLIT-MS and record mass spectra. The mass drift was reduced after the improvement in electronics to stabilize the digital waveform voltage during the mass scan. Tandem mass spectrometry (MS) has been achieved by using digital asymmetric waveform isolation (DAWI), forward and reverse scan, and collision induced dissociation (CID). The isolation and CID efficiency for methyl salicylate were 83.9% and 81.3%, respectively. A novel buffer gas inlet system was designed to enhance the sensitivity and allow easy and safe use of the instrument. Limits of detection below 1 ppbv were obtained for several mixed gaseous samples.

  17. Quantification and confirmation of flunixin in equine plasma by liquid chromatography-quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Luo, Yi; Rudy, Jeffrey A; Uboh, Cornelius E; Soma, Lawrence R; Guan, Fuyu; Enright, James M; Tsang, Deborah S

    2004-03-05

    The method describes quantification and confirmation of flunixin in equine plasma by liquid chromatography-quadrupole time-of-flight mass spectrometry (LC/Q-TOF/MS/MS). Samples were screened by enzyme-linked immunosorbent assay (ELISA) and only those samples presumptively declared positive were subjected to quantification and confirmation for the presence of flunixin by this method. The method is also readily adaptable to instrumental screening for the analyte. Flunixin was recovered from plasma by liquid-liquid extraction (LLE). The sample was diluted with 2 ml saturated phosphate buffer (pH 3.10) prior to LLE. The dried extract was reconstituted in acetonitrile:water:formic acid (50:50:0.1, v/v/v) and subsequently analyzed on a Q-TOF tandem mass spectrometer (Micromass) operated under electrospray ionization positive ion mode. The concentration of flunixin was determined by the internal standard (IS) calibration method using the peak area ratio with clonixin as the IS. The limits of detection (LOD) and quantification (LOQ) for flunixin in equine plasma were 0.1 and 1 ng/ml, respectively, whereas the limit of confirmation (LOC) was 2.5 ng/ml. The qualifying ions for the identification of flunixin were m/z 297 [M+H](+), 279 (BP), 264, 259, 239 and those for clonixin (IS) were m/z 263 [M+H](+), 245 (BP) and 210. The measurement uncertainty about the result was 8.7%. The method is simple, sensitive, robust and reliably fast in the quantification and confirmation of flunixin in equine plasma. Application of this method will assist racing authorities in the enforcement of tolerance plasma concentration of flunixin in the racehorse on race day.

  18. Dynamic mass spectrometer for studies of organic and inorganic molecules

    Energy Technology Data Exchange (ETDEWEB)

    Zavilopulo, A.N. [Institute of Electron Physics, Ukr. Nat. Acad. Sci., Department of Ion Processes, Universytetska Str. 21, 88017 Uzhhorod (Ukraine)]. E-mail: an@zvl.iep.uzhgorod.ua; Shpenik, O.B. [Institute of Electron Physics, Ukr. Nat. Acad. Sci., Department of Ion Processes, Universytetska Str. 21, 88017 Uzhhorod (Ukraine); Surkov, V.A. [SELMI Inc., Sumy (Ukraine)

    2006-07-28

    Experimental technique is described and relative cross-sections of direct and dissociative ionization of CO{sub 2}, C{sub 4}H{sub 9}OH, C{sub 2}H{sub 5}OH, CH{sub 3}OH, C{sub 6}H{sub 12}O{sub 6} and C{sub 7}H{sub 8} molecules by electron impact in the near-threshold energy range are obtained. The experiment is performed on a setup with ion mass separation based on a monopole mass spectrometer which is proved to be successful for such a sort of experiments. For the incident electron energy range from 7 to 35 eV the energy dependences of cross-section of appearance of the main molecule ions and the fragment ions formed due to its dissociation are given.

  19. Multi-collector Isotope Ratio Mass Spectrometer -- Operational Performance Report

    Energy Technology Data Exchange (ETDEWEB)

    Appelhans, Anthony D; Olson, John E; Watrous, Matthew G; Ward, Michael B.; Dahl, David A.

    2010-12-01

    This report describes the operational testing of a new magnetic sector mass spectrometer that utilizes seven full-sized discrete dynode electron multipliers operating simultaneously. The instrument includes a newly developed ion dispersion lens that enables the mass dispersed individual isotope beams to be separated sufficiently to allow a full-sized discrete dynode pulse counting multiplier to be used to measure each isotope beam. The performance of the instrument was measured using SRM 996 (244Pu spike) at loadings of 2.4 and 12 fg on resin beads and with SRM 4350B Columbia River Sediment samples. The measured limit of detection (3s) for 240Pu was 3.4 attograms for SRM 996. The limit of quantitation (LOQ), defined as 10 s, was 11.2 attograms. The measured concentration of 239Pu in the CRS standard was 152 ± 6 fg/g.

  20. Low-Pressure, Field-Ionizing Mass Spectrometer

    Science.gov (United States)

    Hartley, Frank; Smith, Steven

    2009-01-01

    A small mass spectrometer utilizing a miniature field ionization source is now undergoing development. It is designed for use in a variety of applications in which there are requirements for a lightweight, low-power-consumption instrument that can analyze the masses of a wide variety of molecules and ions. The device can operate without need for a high-vacuum, carrier-gas feed radioactive ionizing source, or thermal ionizer. This mass spectrometer can operate either in the natural vacuum of outer space or on Earth at any ambient pressure below 50 torr (below about 6.7 kPa) - a partial vacuum that can easily be reached by use of a small sampling pump. This mass spectrometer also has a large dynamic range - from singly charged small gas ions to deoxyribonucleic acid (DNA) fragments larger than 104 atomic mass units - with sensitivity adequate for detecting some molecules and ions at relative abundances of less than one part per billion. This instrument (see figure) includes a field ionizer integrated with a rotating-field mass spectrometer (RFMS). The field ionizer effects ionization of a type characterized as "soft" in the art because it does not fragment molecules or initiate avalanche arcing. What makes the "soft" ionization mode possible is that the distance between the ionizing electrodes is less than mean free path for ions at the maximum anticipated operating pressure, so that the ionizer always operates on the non-breakdown side of the applicable Paschen curve (a standard plot of breakdown potential on the ordinate and pressure electrode separation on the abscissa). The field ionizer in this instrument is fabricated by micromachining a submicron-thick membrane out of an electrically nonconductive substrate, coating the membrane on both sides to form electrodes, then micromachining small holes through the electrodes and membrane. Because of the submicron electrode separation, even a potential of only 1 V applied between the electrodes gives rise to an electric

  1. Mass measurements on radioactive isotopes with a Penning trap mass spectrometer

    CERN Document Server

    Bollen, G; Audi, G; Beck, D; Herfurth, F; Kluge, H J; Kohl, A; Lunney, M D; Moore, R B; De Saint-Simon, M; Schark, E; Schwarz, S; Szerypo, R B

    1999-01-01

    Penning trap mass measurements on short-lived isotopes are performed with the ISOLTRAP mass spectrometer at the radioactive beam facility ISOLDE/CERN. In the last years the applicability of the spectrometer has been considerably extended by the installation of an RFQ trap ion beam buncher and a new cooler Penning trap, which is operated as an isobar separator. These improvements allowed for the first time measurements on isotopes of rare earth elements and on isotopes with Z=80-85. In all cases an accuracy of $\\delta$m/m approximately =1$\\cdot$10$^{-7}$was achieved. (20 refs).

  2. Calibration of a basic secondary ion mass spectrometer, by means of elastic recoil detection, for hydrogen isotopes implanted into graphite

    Energy Technology Data Exchange (ETDEWEB)

    Paynter, R.W.; Turgeon, S.; Sabet-Sharghi, R.; Leblanc, L.; Pageau, J.F.; Ross, G.G. (INRS-Energie et Materiaux, Varennes, PQ (Canada))

    1992-07-01

    A secondary ion mass spectrometer (SIMS) equipped with a low-resolution argon ion source and a small quadrupole ion mass analyser was calibrated for moderate to high concentrations of hydrogen and deuterium in graphite. The polished graphite samples were implanted with hydrogen isotope ions of 1 or 2 keV energy. The depth profiles of the implanted hydrogen were determined by means of elastic recoil detection (ERD) and compared with those obtained by SIMS. Linear correlations were found between the peak D{sup +}/C{sup +} or CH{sup +}/C{sup +} ratio and the maximum D or H concentration determined by ERD, as well as between the integral of the SIMS profile curves and the total quantity of hydrogen isotope. (author).

  3. Direct mass measurements of neutron-deficient xenon isotopes using the ISOLTRAP mass spectrometer

    CERN Document Server

    Dilling, J; Beck, D; Bollen, G; Herfurth, F; Kellerbauer, A G; Kluge, H J; Moore, R B; Scheidenberger, C; Schwarz, S; Sikler, G

    2004-01-01

    The masses of the noble-gas Xe isotopes with 114 $\\leq$ A $\\leq$ 123 have been directly measured for the first time. The experiments were carried out with the ISOLTRAP triple trap spectrometer at the online mass separator ISOLDE/CERN. A mass resolving power of the Penning trap spectrometer of $m/\\Delta m$ of close to a million was chosen resulting in an accuracy of $\\delta m \\leq 13$ keV for all investigated isotopes. Conflicts with existing, indirectly obtained, mass data by several standard deviations were found and are discussed. An atomic mass evaluation has been performed and the results are compared to information from laser spectroscopy experiments and to recent calculations employing an interacting boson model.

  4. Isotopes of nitrogen on Mars: Atmospheric measurements by Curiosity's mass spectrometer

    Science.gov (United States)

    Wong, Michael H; Atreya, Sushil K; Mahaffy, Paul N; Franz, Heather B; Malespin, Charles; Trainer, Melissa G; Stern, Jennifer C; Conrad, Pamela G; Manning, Heidi L K; Pepin, Robert O; Becker, Richard H; McKay, Christopher P; Owen, Tobias C; Navarro-González, Rafael; Jones, John H; Jakosky, Bruce M; Steele, Andrew

    2013-01-01

    [1] The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) measured a Mars atmospheric14N/15N ratio of 173 ± 11 on sol 341 of the mission, agreeing with Viking's measurement of 168 ± 17. The MSL/SAM value was based on Quadrupole Mass Spectrometer measurements of an enriched atmospheric sample, with CO2 and H2O removed. Doubly ionized nitrogen data at m/z 14 and 14.5 had the highest signal/background ratio, with results confirmed by m/z 28 and 29 data. Gases in SNC meteorite glasses have been interpreted as mixtures containing a Martian atmospheric component, based partly on distinctive14N/15N and40Ar/14N ratios. Recent MSL/SAM measurements of the40Ar/14N ratio (0.51 ± 0.01) are incompatible with the Viking ratio (0.35 ± 0.08). The meteorite mixing line is more consistent with the atmospheric composition measured by Viking than by MSL. PMID:26074632

  5. A Generic Multiple Reaction Monitoring Based Approach for Plant Flavonoids Profiling Using a Triple Quadrupole Linear Ion Trap Mass Spectrometry

    Science.gov (United States)

    Yan, Zhixiang; Lin, Ge; Ye, Yang; Wang, Yitao; Yan, Ru

    2014-06-01

    Flavonoids are one of the largest classes of plant secondary metabolites serving a variety of functions in plants and associating with a number of health benefits for humans. Typically, they are co-identified with many other secondary metabolites using untargeted metabolomics. The limited data quality of untargeted workflow calls for a shift from the breadth-first to the depth-first screening strategy when a specific biosynthetic pathway is focused on. Here we introduce a generic multiple reaction monitoring (MRM)-based approach for flavonoids profiling in plants using a hybrid triple quadrupole linear ion trap (QTrap) mass spectrometer. The approach includes four steps: (1) preliminary profiling of major aglycones by multiple ion monitoring triggered enhanced product ion scan (MIM-EPI); (2) glycones profiling by precursor ion triggered EPI scan (PI-EPI) of major aglycones; (3) comprehensive aglycones profiling by combining MIM-EPI and neutral loss triggered EPI scan (NL-EPI) of major glycone; (4) in-depth flavonoids profiling by MRM-EPI with elaborated MRM transitions. Particularly, incorporation of the NH3 loss and sugar elimination proved to be very informative and confirmative for flavonoids screening. This approach was applied for profiling flavonoids in Astragali radix ( Huangqi), a famous herb widely used for medicinal and nutritional purposes in China. In total, 421 flavonoids were tentatively characterized, among which less than 40 have been previously reported in this medicinal plant. This MRM-based approach provides versatility and sensitivity that required for flavonoids profiling in plants and serves as a useful tool for plant metabolomics.

  6. Effect of heating strategies on whey protein denaturation--Revisited by liquid chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Akkerman, M; Rauh, V M; Christensen, M; Johansen, L B; Hammershøj, M; Larsen, L B

    2016-01-01

    Previous standards in the area of effect of heat treatment processes on milk protein denaturation were based primarily on laboratory-scale analysis and determination of denaturation degrees by, for example, electrophoresis. In this study, whey protein denaturation was revisited by pilot-scale heating strategies and liquid chromatography quadrupole time-of-flight mass spectrometer (LC/MC Q-TOF) analysis. Skim milk was heat treated by the use of 3 heating strategies, namely plate heat exchanger (PHE), tubular heat exchanger (THE), and direct steam injection (DSI), under various heating temperatures (T) and holding times. The effect of heating strategy on the degree of denaturation of β-lactoglobulin and α-lactalbumin was determined using LC/MC Q-TOF of pH 4.5-soluble whey proteins. Furthermore, effect of heating strategy on the rennet-induced coagulation properties was studied by oscillatory rheometry. In addition, rennet-induced coagulation of heat-treated micellar casein concentrate subjected to PHE was studied. For skim milk, the whey protein denaturation increased significantly as T and holding time increased, regardless of heating method. High denaturation degrees were obtained for T >100°C using PHE and THE, whereas DSI resulted in significantly lower denaturation degrees, compared with PHE and THE. Rennet coagulation properties were impaired by increased T and holding time regardless of heating method, although DSI resulted in less impairment compared with PHE and THE. No significant difference was found between THE and PHE for effect on rennet coagulation time, whereas the curd firming rate was significantly larger for THE compared with PHE. Micellar casein concentrate possessed improved rennet coagulation properties compared with skim milk receiving equal heat treatment.

  7. Electrospray ionization quadrupole time-of-flight tandem mass spectrometric analysis of hexamethylenediamine-modified maltodextrin and dextran

    NARCIS (Netherlands)

    Sisu, E.; Bosker, W.T.E.; Norde, W.; Slaghek, T.M.; Timmermans, J.W.; Peter-Katalinić, J.; Cohen-Stuart, M.A.; Zamfir, A.D.

    2006-01-01

    A combined methodology for obtaining at the preparative scale and characterization by nanoelectrospray ionization (nanoESI) quadrupole time-of-flight (QTOF) mass spectrometry (MS) and tandem MS (MS/MS) of linear polysaccharides modified at the reducing end is presented. Two polydisperse maltodextrin

  8. A chemical ionization mass spectrometer for continuous underway shipboard analysis of dimethylsulfide in near-surface seawater

    Directory of Open Access Journals (Sweden)

    E. S. Saltzman

    2009-11-01

    Full Text Available A compact, low-cost atmospheric pressure, chemical ionization mass spectrometer ("mini-CIMS" has been developed for continuous underway shipboard measurements of dimethylsulfide (DMS in seawater. The instrument was used to analyze DMS in air equilibrated with flowing seawater across a porous Teflon membrane equilibrator. The equilibrated gas stream was diluted with air containing an isotopically-labeled internal standard. DMS is ionized at atmospheric pressure via proton transfer from water vapor, then declustered, mass filtered via quadrupole mass spectrometry, and detected with an electron multiplier. The instrument described here is based on a low-cost residual gas analyzer (Stanford Research Systems, which has been modified for use as a chemical ionization mass spectrometer. The mini-CIMS has a gas phase detection limit of 220 ppt DMS for a 1 min averaging time, which is roughly equivalent to a seawater DMS concentration of 0.1 nM DMS at 20°C. The mini-CIMS has the sensitivity, selectivity, and time response required for underway measurements of surface ocean DMS over the full range of oceanographic conditions. The simple, robust design and relatively low cost of the instrument are intended to facilitate use in process studies and surveys, with potential for long-term deployment on research vessels, ships of opportunity, and large buoys.

  9. A chemical ionization mass spectrometer for continuous underway shipboard analysis of dimethylsulfide in near-surface seawater

    Directory of Open Access Journals (Sweden)

    E. S. Saltzman

    2009-07-01

    Full Text Available A compact, low-cost atmospheric pressure, chemical ionization mass spectrometer ("mini-CIMS" has been developed for continuous underway shipboard measurements of dimethylsulfide (DMS in seawater. The instrument was used to analyze DMS in air equilibrated with flowing seawater across a porous Teflon membrane equilibrator. The equilibrated gas stream was diluted with air containing an isotopically-labeled internal standard. DMS is ionized at atmospheric pressure via proton transfer from water vapor, then declustered, mass filtered via quadrupole mass spectrometry, and detected with an electron multiplier. The instrument described here is based on a low-cost residual gas analyzer (Stanford Research Systems, which has been modified for use as a chemical ionization mass spectrometer. The mini-CIMS has a gas phase detection limit of 170 ppt DMS for a 1 min averaging time, which is roughly equivalent to a seawater DMS concentration of 0.1 nM DMS at 20°C. The mini-CIMS has the sensitivity, selectivity, and time response required for underway measurements of surface ocean DMS over the full range of oceanographic conditions. The simple, robust design and relatively low cost of the instrument are intended to facilitate use in process studies and surveys, with potential for long-term deployment on research vessels, ships of opportunity, and large buoys.

  10. High mass resolution time of flight mass spectrometer for measuring products in heterogeneous catalysis in highly sensitive microreactors

    DEFF Research Database (Denmark)

    Andersen, Thomas; Jensen, Robert; Christensen, M. K.

    2012-01-01

    response. Gas analysis is performed with a time of flight mass spectrometer with a modified nude Bayard-Alpert ionization gauge as gas ionization source. The mass resolution of the time of flight mass spectrometer using the ion gauge as ionization source is estimated to m∕Δm > 2500. The system design...

  11. Diagnostics aid for mass spectrometer trouble-shooting

    Science.gov (United States)

    Filby, E. E.; Rankin, R. A.; Webb, G. W.

    The MS Expert system provides problem diagnostics for instruments used in the Mass Spectrometry Laboratory (MSL). The most critical results generated on these mass spectrometers are the uranium concentration and isotopic content data used for process control and materials accountability at the Idaho Chemical Processing Plant. The two purposes of the system are: (1) to minimize instrument downtime and thereby provide the best possible support to the Plant, and (2) to improve long-term data quality. This system combines the knowledge of several experts on mass spectrometry to provide a diagnostic tool, and can make these skills available on a more timely basis. It integrates code written in the Pascal language with a knowledge base entered into a commercial expert system shell. The user performs some preliminary status checks, and then selects from among several broad diagnostic categories. These initial steps provide input to the rule base. The overall analysis provides the user with a set of possible solutions to the observed problems, graded as to their probabilities. Besides the trouble-shooting benefits expected from this system, it will also provide structures diagnostic training for lab personnel. In addition, development of the system knowledge base has already produced a better understanding of instrument behavior. Two key findings are that a good user interface is necessary for full acceptance of the tool, and a development system should include standard programming capabilities as well as the expert system shell.

  12. Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

    Science.gov (United States)

    Wolf, Ruth E.; Adams, Monique

    2015-01-01

    Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

  13. Liquid chromatography with triple-quadrupole or quadrupole-time of flight mass spectrometry for screening and confirmation of residues of pharmaceuticals in water.

    Science.gov (United States)

    Stolker, Alida A M; Niesing, Willem; Hogendoorn, Elbert A; Versteegh, Johanna F M; Fuchs, Regine; Brinkman, Udo A Th

    2004-02-01

    LC-MS-MS has been performed with triple-quadrupole (QqQ) and quadrupole-time of flight (Q-ToF) instruments and has been used for screening and confirmation of pharmaceuticals in surface, drinking, and ground water. Screening was based on monitoring of one specific MS-MS ion of the target compounds. Confirmation of the identity of the pharmaceuticals was based either on the monitoring of two specific MS-MS ions and calculation of the ratio of their intensities, or on the exact masses of MS-MS product ions obtained for a molecular ion by use of LC-Q-ToF MS. The set of pharmaceuticals included four analgesics (acetylsalicylic acid, diclofenac, ibuprofen, and paracetamol), three antibiotics (sulfamethoxazole, erythromycin, and chloramphenicol), five blood-lipid regulators and beta-blockers (fenofibrate, bezafibrate, clofibric acid, bisoprolol, and metoprolol), and the anti-epileptic drug carbamazepine. Limits of quantification ranged from 5 to 25 ng L(-1). Fifty-six samples were analysed and residues of the pharmaceuticals were detected in almost all surface and groundwater and in some drinking water samples. The identity of the compounds could be confirmed by use of both QqQ- and Q-ToF-based LC-MS-MS. However, the latter technique has the distinct advantage that a large number of pharmaceuticals can be screened and confirmed at low concentrations (1-100 ng L(-1)) in one run.

  14. Quantification of intermediate-abundance proteins in serum by multiple reaction monitoring mass spectrometry in a single-quadrupole ion trap.

    Science.gov (United States)

    Lin, Shanhua; Shaler, Thomas A; Becker, Christopher H

    2006-08-15

    A method is presented to quantify intermediate-abundance proteins in human serum using a single-quadrupole linear ion trap mass spectrometer-in contrast, for example, to a triple-quadrupole mass spectrometer. Stable-isotope-labeled (tryptic) peptides are spiked into digested protein samples as internal standards, aligned with the traditional isotope dilution approach. As a proof-of-concept experiment, four proteins of intermediate abundance were selected, coagulation factor V, adiponectin, C-reactive protein (CRP), and thyroxine binding globulin. Stable-isotope-labeled peptides were synthesized with one tryptic sequence from each of these proteins. The normal human serum concentration ranges of these proteins are from 1 to 30 microg/mL (or 20 to 650 pmol/mL). These labeled peptides and their endogenous counterparts were analyzed by LC-MS/MS using multiple reaction monitoring, a multiplexed form of the selected reaction monitoring technique. For these experiments, only one chromatographic dimension (on-line reversed-phase capillary column) was used. Improved limits of detection will result with multidimensional chromatographic methods utilizing more material per sample. Standard curves of the spiked calibrants were generated with concentrations ranging from 3 to 700 pmol/mL using both neat solutions and peptides spiked into the complex matrix of digested serum protein solution where ion suppression effects and interferences are common. Endogenous protein concentrations were determined by comparing MS/MS peak areas of the endogenous peptides to the isotopically labeled internal calibrants. The derived concentrations from a normal human serum pool (neglecting loss of material during sample processing) were 9.2, 110, 120, and 246 pmol/mL for coagulation factor V, adiponectin, CRP, and thyroxine binding globulin, respectively. These concentrations generally agree with the reported normal ranges for these proteins. As a measure of analytical reproducibility of this

  15. Degradation study of enniatins by liquid chromatography-triple quadrupole linear ion trap mass spectrometry.

    Science.gov (United States)

    Serrano, A B; Meca, G; Font, G; Ferrer, E

    2013-12-15

    Enniatins A, A1, B and B1 (ENs) are mycotoxins produced by Fusarium spp. and are normal contaminants of cereals and derivate products. In this study, the stability of ENs was evaluated during food processing by simulation of pasta cooking. Thermal treatments at different incubation times (5, 10 and 15 min) and different pH (4, 7 and 10) were applied in an aqueous system and pasta resembling system (PRS). The concentrations of the targeted mycotoxins were determined using liquid chromatography coupled to tandem mass spectrometry. High percentages of ENs reduction (81-100%) were evidenced in the PRS after the treatments at 5, 10 and 15 min of incubation. In contrast to the PRS, an important reduction of the ENs was obtained in the aqueous system after 15 min of incubation (82-100%). In general, no significant differences were observed between acid, neutral and basic solutions. Finally, several ENs degradation products were identified using the technique of liquid chromatography-triple quadrupole linear ion trap mass spectrometry.

  16. Quadrupole magnetic mapping of the high resolution spectrometers of Thomas Jefferson National Accelerator Laboratory, Hall A. (Q.M.M. project: Quadrupole Magnetic Measurement); Cartographie magnetique des quadripoles des spectrometre a haute resolution du Thomas Jefferson National Accelerator Laboratory, Hall A. (Le projet Q.M.M.: Quadrupole Magnetic Measurement)

    Energy Technology Data Exchange (ETDEWEB)

    Quemener, Gilles [Ecole Doctorale des Science Fondamentales, Universite Blaise Pascal, U.F.R. de Recherche Scientifique et Technique, F-63177 Aubiere Cedex (France)

    1997-12-19

    This thesis describes the magnetic measurements that have been performed on the superconducting quadrupoles of the High Resolution Spectrometers of TJNAF, Hall A (USA), which are designed to measure particle momentum up to 4 GeV.c{sup -1} with a {sigma}p/p = 10{sup -4} resolution. The mapping method is based on rotating coil technique, the originality being a segmentation of the probe along the quad axis. Together with an accurate magnet modelling, the measurement of the flux variations through the set of rotating coils allows to determine the magnetic field at each point. We use the 3D field formalism, i.e., the Fourier-Bessel expansion of the field obtained by solving the Laplace equation. We describe the QMM method and then the apparatus consisting in two probes of length 1.6 m and 3.2 m built to map the three quadrupoles Q1, Q2, Q3. Data processing uses Fourier analysis. The mapping of the Electron Arm took place in situ in 1996. A first set of results concerns integral measurements including the properties of excitation cycle of the magnets (saturation and hysteresis). Second set of results in terms of local field yields the 3D field maps of the quadrupoles. After having applied corrections to the data we obtain a local field accuracy of 5 Gauss on each component, i.e. an uncertainty of 5.10{sup -4} relative to the quadrupole central field. We use SNAKE ray-tracing code with the implementation of QMM field maps and obtain preliminary results on HRS optics. (author) 48 refs., 93 figs., 41 tabs.

  17. 21 Tesla Fourier Transform Ion Cyclotron Resonance Mass Spectrometer Greatly Expands Mass Spectrometry Toolbox

    Science.gov (United States)

    Shaw, Jared B.; Lin, Tzu-Yung; Leach, Franklin E.; Tolmachev, Aleksey V.; Tolić, Nikola; Robinson, Errol W.; Koppenaal, David W.; Paša-Tolić, Ljiljana

    2016-12-01

    We provide the initial performance evaluation of a 21 Tesla Fourier transform ion cyclotron resonance mass spectrometer operating at the Environmental Molecular Sciences Laboratory at the Pacific Northwest National Laboratory. The spectrometer constructed for the 21T system employs a commercial dual linear ion trap mass spectrometer coupled to a FTICR spectrometer designed and built in-house. Performance gains from moving to higher magnetic field strength are exemplified by the measurement of peptide isotopic fine structure, complex natural organic matter mixtures, and large proteins. Accurate determination of isotopic fine structure was demonstrated for doubly charged Substance P with minimal spectral averaging, and 8158 molecular formulas assigned to Suwannee River Fulvic Acid standard with root-mean-square (RMS) error of 10 ppb. We also demonstrated superior performance for intact proteins; namely, broadband isotopic resolution of the entire charge state distribution of apo-transferrin (78 kDa) and facile isotopic resolution of monoclonal antibody under a variety of acquisition parameters (e.g., 6 s time-domains with absorption mode processing yielded resolution of approximately 1 M at m/z = 2700).

  18. 21 Tesla Fourier Transform Ion Cyclotron Resonance Mass Spectrometer Greatly Expands Mass Spectrometry Toolbox

    Energy Technology Data Exchange (ETDEWEB)

    Shaw, Jared B.; Lin, Tzu-Yung; Leach, Franklin E.; Tolmachev, Aleksey V.; Tolić, Nikola; Robinson, Errol W.; Koppenaal, David W.; Paša-Tolić, Ljiljana

    2016-10-12

    We provide the initial performance evaluation of a 21 Tesla Fourier transform ion cyclotron resonance mass spectrometer operating at the Environmental Molecular Sciences Laboratory at Pacific Northwest National Laboratory. The spectrometer constructed for the 21T system employs a commercial dual linear ion trap mass spectrometer coupled to a FTICR spectrometer designed and built in-house. Performance gains from moving to higher magnetic field strength are exemplified by the measurement of peptide isotopic fine structure, complex natural organic matter mixtures, and large proteins. Accurate determination of isotopic fine structure was demonstrated for doubly charged substance P with minimal spectral averaging, and 8,158 molecular formulas assigned to Suwannee River Fulvic Acid standard with RMS error of 10 ppb. We also demonstrated superior performance for intact proteins; namely, broadband isotopic resolution of the entire charge state distribution of apotransferrin (78 kDa) and facile isotopic resolution of monoclonal antibody under a variety of acquisition parameters (e.g. 6 s time-domains with absorption mode processing yielded resolution of approximately 1M at m/z =2,700).

  19. Comparison of a triple-quadrupole and a quadrupole time-of-flight mass analyzer to quantify 16 opioids in human plasma.

    Science.gov (United States)

    Viaene, Johan; Lanckmans, Katrien; Dejaegher, Bieke; Mangelings, Debby; Vander Heyden, Yvan

    2016-08-05

    The aim of this work is to study whether a quadrupole time-of-flight (QToF) mass analyzer, coupled to an ultra high performance liquid chromatography (UHPLC) system, can be a valuable alternative for a triple-quadrupole (QqQ) mass analyzer, for quantitative toxicological purposes. The case study considered was the quantification of 16 opioids (6-monoacetylmorphine, buprenorphine, codeine, dihydrocodeine, ethylmorphine, fentanyl, hydrocodone, hydromorphone, morphine, norbuprenorphine, norcodeine, norfentanyl, oxycodone, oxymorphone, pholcodine and tilidine) in human plasma. Both methods were validated in parallel in terms of selectivity, matrix effects, extraction recovery, carry-over, bias, precision and sensitivity. Accuracy-profile methodology was used to determine the optimal calibration model, and to estimate bias, repeatability, intermediate precision and total error. Selectivity was demonstrated for all opioids and deuterated analogues, except for codeine-d3 on the UHPLC-QTOF. For most compounds, extraction recoveries were in the range 60 to 80% on both systems, except for the synthetic analogues, buprenorphine, fentanyl and tilidine, where large variability is observed. Carry-over was negligible on both systems. For different opioids, the optimal calibration model was different between the systems. The accuracy profiles of the majority of the opioids indicated that, over the entire tested concentration range, for more than 5% of the future measurements, total errors are expected to exceed the a priori defined 15% acceptance limit. For some exceptions, however, the measurements even suffer from total errors above 30%, which can be attributed to the solid phase extraction procedure that was applied as sample pretreatment technique. Sensitivity was generally tenfold better on the LC-QToF system, probably due to the difference in ion choice for quantification between both systems. In conclusion, the best performing system seemed to depend on the compound, on the

  20. A field-deployable, chemical ionization time-of-flight mass spectrometer

    Directory of Open Access Journals (Sweden)

    T. H. Bertram

    2011-07-01

    Full Text Available We constructed a new chemical ionization time-of-flight mass spectrometer (CI-TOFMS that measures atmospheric trace gases in real time with high sensitivity. We apply the technique to the measurement of formic acid via negative-ion proton transfer, using acetate as the reagent ion. A novel high pressure interface, incorporating two RF-only quadrupoles is used to efficiently focus ions through four stages of differential pumping before analysis with a compact TOFMS. The high ion-duty cycle (>20 % of the TOFMS combined with the efficient production and transmission of ions in the high pressure interface results in a highly sensitive (>300 ions s−1 pptv−1 formic acid instrument capable of measuring and saving complete mass spectra at rates faster than 10 Hz. We demonstrate the efficient transfer and detection of both bare ions and ion-molecule clusters, and characterize the instrument during field measurements aboard the R/V Atlantis as part of the CalNex campaign during the spring of 2010. The in-field short-term precision is better than 5 % at 1 pptv (pL/L, for 1-s averages. The detection limit (3 σ, 1-s averages of the current version of the CI-TOFMS, as applied to the in situ detection of formic acid, is limited by the magnitude and variability in the background determination and was determined to be 4 pptv. Application of the CI-TOFMS to the detection of other inorganic and organic acids, as well as the use of different reagent ion molecules (e.g. I, CF3O, CO3 is promising, as we have demonstrated efficient transmission and detection of both bare ions and their associated ion-molecule clusters.

  1. High-precision masses of neutron-deficient rubidium isotopes using a Penning trap mass spectrometer

    CERN Document Server

    Kellerbauer, A G; Beck, D; Blaum, K; Bollen, G; Guénaut, C; Herfurth, F; Herlert, A; Kluge, H J; Lunney, D; Schwarz, S; Schweikhard, L; Weber, C; Yazidjian, C

    2007-01-01

    The atomic masses of the neutron-deficient radioactive rubidium isotopes $^{74-77,79,80,83}$Rb have been measured with the Penning trap mass spectrometer ISOLTRAP. Using the time-of-flight cyclotron resonance technique, relative mass uncertainties ranging from $1.6 \\times 10^{-8}$ to $5.6 \\times 10^{-8}$ were achieved. In all cases, the mass precision was significantly improved as compared with the prior Atomic-Mass Evaluation; no significant deviations from the literature values were observed. The exotic nuclide $^{74}$Rb with a half-life of only 65 ms, is the shortest-lived nuclide on which a high-precision mass measurement in a Penning trap has been carried out. The significance of these measurements for a check of the conserved-vector-current hypothesis of the weak interaction and the unitarity of the Cabibbo-Kobayashi-Maskawa matrix is discussed.

  2. Quantification of 2'-deoxy-2'-β-fluoro-4'-azidocytidine in rat and dog plasma using liquid chromatography-quadrupole time-of-flight and liquid chromatography-triple quadrupole mass spectrometry: Application to bioavailability and pharmacokinetic studies.

    Science.gov (United States)

    Peng, Youmei; Cheng, Tiefeng; Dong, Lihong; Zhang, Yuhai; Chen, Xiaojing; Jiang, Jinhua; Zhang, Jingmin; Guo, Xiaohe; Guo, Mintong; Chang, Junbiao; Wang, Qingduan

    2014-09-01

    2'-Deoxy-2'-β-fluoro-4'-azidocytidine (FNC) is a novel pyrimidine analog that inhibits not only the replication of the hepatitis B virus (HBV), hepatitis C virus (HCV) and HIV but also the replication of lamivudine-resistant HBV, 4'-azidocytidine or 2'-β-methylcytidine-resistant HCV, and nucleoside reverse-transcriptase inhibitor-resistant HIV variants. The present study was undertaken to evaluate the absolute oral bioavailability of FNC in rats and the pharmacokinetic properties of FNC after intragastric administration of single and multiple doses in rats and dogs. A sensitive high-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (HPLC/Q-TOF MS) method and a reliable high-performance liquid chromatography tandem triple quadrupole mass spectrometry (HPLC/QqQ MS/MS) method were established for the determination of FNC in the rat and dog plasmas, respectively. The sample preparation involved a protein-precipitation method with methanol after the addition of lamivudine as an internal standard. FNC was analyzed by LC using a YMC-Pack Pro C18 column (150mm×4.6mm, 3μm) with methanol (containing 0.3% formic acid): 10mM ammonium acetate (containing 0.3% formic acid, pH 2.8) (35:65, v/v) as the mobile phase. Both mass spectrometers were equipped with an electrospray ionization interface in the positive-ion mode. The linear range was from 2.00 to 2000.00ngmL(-1) in rat plasma and 0.50 to 400.00ngmL(-1) in dog plasma. The intraday and interday precision were less than 10.55%, and the accuracy was in the range of -5.86 to 5.13%. The mean recoveries were greater than 82.70% and 82.97% for FNC and IS, respectively. The HPLC/Q-TOF MS and HPLC/QqQ MS/MS methods were both successfully applied in the pharmacokinetic studies of FNC in rats and dogs.

  3. Metabolite Profile of Salidroside in Rats by Ultraperformance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry and High-Performance Liquid Chromatography Coupled with Quadrupole-Linear Ion Trap Mass Spectrometry.

    Science.gov (United States)

    Hu, Zhiwei; Wang, Ziming; Liu, Yong; Wu, Yan; Han, Xuejiao; Zheng, Jian; Yan, Xiufeng; Wang, Yang

    2015-10-21

    In the present work, the salidroside metabolite profile in rat urine was investigated, and subsequently the metabolic pathways of salidroside were proposed. After administrations of salidroside at an oral dose of 100 or 500 mg/kg, rat urine samples were collected and pretreated with methanol to precipitate the proteins. The pretreated samples were analyzed by an Acquity ultraperformance liquid chromatography (UPLC) coupled with an HSS T3 column and detected by quadrupole time-of-flight mass spectrometry (Q-TOF-MS) or high-performance liquid chromatography coupled with hybrid triple-quadrupole linear ion trap mass spectrometry (HPLC/Q-trap-MS). A total of eight metabolites were detected and identified on the basis of the characteristics of their protonated ions in the urine samples. The results elucidated that salidroside was metabolized via glucuronidation, sulfation, deglycosylation, hydroxylation, methylation, and dehydroxylation pathways in vivo.

  4. Analysis of coffee bean extracts by use of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    O'Driscoll, Daniel James

    2014-01-01

    The number of flavour chemicals identified in coffee has reached over 1000 [1], [2]. Coffee is one of the world's most popular beverages [3], highly studied for its health-related properties [4], [5], [6]. Studies on coffee associated with human health have focused on the negative aspects, such as the toxicity of caffeine [7], [8]. Complex chemistry happens during coffee roasting and according to the literature, a number of compounds have been detected and quantified in coffee beans samples by UPLC-Q-TOF/MS [9], [10], [11], [12]. The following method offers a simple approach for the qualitative and quantitative analysis of coffee bean extracts using a Waters Acquity G2 UPLC-Q-TOF/MS instrument adapted from the method by Kenny et al., [12]. The following modifications were made:•The method by Kenny et al. was developed on a triple quadrupole mass spectrometer, the below method was developed on a Q-TOF MS.•A combination of utilising both base peak index and mass extraction at 0.05 Da allows for a sensitive, quantitative technique amidst poor background noise and poor separation with high mass accuracy (<5 ppm).•By use of MS(E) centroid experiment, greater mass spectral information for metabolite profiling could be obtained.

  5. Low mass dimuon production with the ALICE muon spectrometer

    CERN Document Server

    Casula, Ester Anna Rita

    Low mass vector meson ($\\rho$, $\\omega$, $\\phi$) production provides key information on the hot and dense state of strongly interacting matter produced in high-energy heavy ion collisions (called Quark Gluon Plasma). Strangeness enhancement is one of the possible signatures of the Quark Gluon Plasma formation and can be accessed through the measurement of $\\phi$ meson production with respect to $\\rho$ and $\\omega$ mesons, while the measurement of the $\\phi$ nuclear modification factor provides a powerful tool to probe the production dynamics and hadronization process in relativistic heavy ion collisions. Vector mesons can be detected through their decays into muon pairs with the ALICE muon spectrometer. This thesis presents the results on the measurement of the $\\phi$ differential cross section, as a function of the transverse momentum, in pp collisions at $\\sqrt{s}$ = 2.76 TeV; the measurement of the $\\phi$ yield and of the nuclear modification factor $R_{pA}$ at forward and backward rapidity, as a function...

  6. Liquid chromatography quadrupole time-of-flight mass spectrometry selective determination of ochratoxin A in wine.

    Science.gov (United States)

    Rodríguez-Cabo, T; Rodríguez, I; Ramil, M; Cela, R

    2016-05-15

    The performance of liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for ochratoxin A (OTA) determination in wine is evaluated for the first time. Sample preparation was optimized to obtain quantitative recoveries at the same time that the efficiency of electrospray ionization (ESI) remained unaltered between sample extracts and calibration standards. Under final conditions, samples (20 mL) were concentrated using a reversed-phase solid-phase extraction (SPE) cartridge, followed by OTA elution with 1 mL of ethyl acetate. The absolute recoveries of the method, established against calibration standards, were 91-121% and 90-113% (without and with internal standard correction, respectively), for wines fortified at 3 concentration levels. The attained LOQ (0.05 ng mL(-1)) remained below the maximum permitted OTA concentration (2 ng mL(-1)) in dry wines. The method was applied to different samples, with OTA being found in some dessert wines at concentrations below 1 ng mL(-1). The ethyl ester of OTA (OTC) could be identified in the same wine samples from its accurate full product ion spectra.

  7. Design and Fabrication of Quadrupole Ion Mass Spectrometer for Upper Atmosphere.

    Science.gov (United States)

    1981-09-30

    Lever arm. 7 Hinge Bracket. 8 Tie down plate. 9 Pivot pin . 10 Aperture cover. 11 Squib shield bracket. 12 Rod spacers. 13 Target insulator. 14 Support...sheet metal truncated cone piece brazed to a cylindrical ring was designed and fabricated. The front plates of four existing LASSII housings were

  8. SCAPS, a two-dimensional ion detector for mass spectrometer

    Science.gov (United States)

    Yurimoto, Hisayoshi

    2014-05-01

    Faraday Cup (FC) and electron multiplier (EM) are of the most popular ion detector for mass spectrometer. FC is used for high-count-rate ion measurements and EM can detect from single ion. However, FC is difficult to detect lower intensities less than kilo-cps, and EM loses ion counts higher than Mega-cps. Thus, FC and EM are used complementary each other, but they both belong to zero-dimensional detector. On the other hand, micro channel plate (MCP) is a popular ion signal amplifier with two-dimensional capability, but additional detection system must be attached to detect the amplified signals. Two-dimensional readout for the MCP signals, however, have not achieve the level of FC and EM systems. A stacked CMOS active pixel sensor (SCAPS) has been developed to detect two-dimensional ion variations for a spatial area using semiconductor technology [1-8]. The SCAPS is an integrated type multi-detector, which is different from EM and FC, and is composed of more than 500×500 pixels (micro-detectors) for imaging of cm-area with a pixel of less than 20 µm in square. The SCAPS can be detected from single ion to 100 kilo-count ions per one pixel. Thus, SCAPS can be accumulated up to several giga-count ions for total pixels, i.e. for total imaging area. The SCAPS has been applied to stigmatic ion optics of secondary ion mass spectrometer, as a detector of isotope microscope [9]. The isotope microscope has capabilities of quantitative isotope images of hundred-micrometer area on a sample with sub-micrometer resolution and permil precision, and of two-dimensional mass spectrum on cm-scale of mass dispersion plane of a sector magnet with ten-micrometer resolution. The performance has been applied to two-dimensional isotope spatial distribution for mainly hydrogen, carbon, nitrogen and oxygen of natural (extra-terrestrial and terrestrial) samples and samples simulated natural processes [e.g. 10-17]. References: [1] Matsumoto, K., et al. (1993) IEEE Trans. Electron Dev. 40

  9. Continuous Measurements of Dissolved Ne, Ar, Kr, and Xe Ratios with a Field-Deployable Gas Equilibration Mass Spectrometer.

    Science.gov (United States)

    Manning, Cara C; Stanley, Rachel H R; Lott, Dempsey E

    2016-03-15

    Noble gases dissolved in natural waters are useful tracers for quantifying physical processes. Here, we describe a field-deployable gas equilibration mass spectrometer (GEMS) that provides continuous, real-time measurements of Ne, Ar, Kr, and Xe mole ratios in natural waters. Gas is equilibrated with a membrane contactor cartridge and measured with a quadrupole mass spectrometer, after in-line purification with reactive metal alloy getters. We use an electron energy of 35 V for Ne to eliminate isobaric interferences, and a higher electron energy for the other gases to improve sensitivity. The precision is 0.7% or better and 1.0% or better for all mole ratios when the instrument is installed in a temperature-controlled environment and a variable-temperature environment, respectively. In the lab, the accuracy is 0.9% or better for all gas ratios using air as the only calibration standard. In the field (and/or at greater levels of disequilbrium), the accuracy is 0.7% or better for Ne/Kr, Ne/Ar, and Ar/Kr, and 2.5% or better for Ne/Xe, Ar/Xe, and Kr/Xe using air as the only calibration standard. The field accuracy improves to 0.6% or better for Ne/Xe, Ar/Xe, and Kr/Xe when the data is calibrated using discrete water samples run on a laboratory-based mass spectrometer. The e-folding response time is 90-410 s. This instrument enables the collection of a large number of continuous, high-precision and accuracy noble gas measurements at substantially reduced cost and labor compared to traditional methods.

  10. [Determination of aflatoxins in cereals and oils by liquid chromatography-triple quadrupole tandem mass spectrometry].

    Science.gov (United States)

    Wang, Xiupin; Li, Peiwu; Yang, Yang; Zhang, Wen; Zhang, Qi; Fan, Sufang; Yu, Li; Wang, Lin; Chen, Xiaomei; Li, Ying; Jiang, Jun

    2011-06-01

    The high performance liquid chromatography (HPLC)-triple quadrupole tandem mass spectrometry was applied for the determination of the aflatoxins: B1 (AFB1), B2 (AFB2), G1 (AFG1) and G2 (AFG2), in cereals and oils. The samples were first extracted by ultrasonic method. The optimized conditions of ultrasonic extraction were as follows: temperature of 50 degrees C, extraction time of 3 min, methanol-water (containing 40 g/L NaCl) (80: 20, v/v) solution as the medium and a ratio of sample to solvent of 1 : 3 (g: mL). The extracts were then purified using an immunoaffinity column. The separation was performed on a C18 column with mobile phases of 10 mmol/L ammonium acetate and methanol in gradient elution. The sensitive detection of the four AFT compounds by electrospray ionization mass spectrometry (ESI-MS) was carried out in selected reaction monitoring (SRM) mode with aflatoxin M1 (AFM1) as the internal standard. Under the optimized conditions, the limits of detection of AFB1, AFB2, AFG1 and AFG2 were 0.002, 0.004, 0.004 and 0.012 microg/kg, respectively. The recoveries of aflatoxins in different spiked cereals and oils were in the range from 87% to 111%. The intra-day and inter-day precisions were not more than 6.7% and 5.6%, respectively. In comparison with the external standard method, this method can effectively inhibit the matrix effects, and greatly improve the accuracy.

  11. Identification of in vitro metabolites of ethylphenidate by liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

    OpenAIRE

    Negreira, Noelia; Erratico, Claudio; Nuijs, van, Alexander L.N.; Covaci, Adrian

    2016-01-01

    Abstract: Ethylphenidate is a new potent synthetic psychoactive drug, structurally related to methylphenidate. Using human liver microsomes and cytosol, we have investigated for the first time the Phase-I and Phase-II in vitro metabolism of ethylphenidate. The structure of the metabolites was elucidated by hybrid quadrupole time-of-flight mass spectrometry. Overall, seven Phase-I, but no Phase-II metabolites were detected. Ethylphenidate underwent hydroxylation forming two primary mono-hydrox...

  12. Application of inductively coupled plasma quadrupole mass spectrometry for the determination of monazite ages by lead isotope ratios

    OpenAIRE

    Godoy,José Marcus; Godoy,Maria Luiza D. P; Aronne,Cláudia C.

    2007-01-01

    In order to evaluate the applicability of inductively coupled plasma quadrupole mass spectrometry to the determination of Pb/Pb, U/Pb and Th/Pb ages of monazite, studies were carried out initially applying lead atom ratio reference standards (NIST SRM 981 and 982). Further, the optimized methodology was applied to monazite sands from three different sites, Sugar Loaf Hill (Rio de Janeiro city), Buena (Rio de Janeiro state) and Black Sands Beach (Guarapari, Espirito Santo state); the obtained ...

  13. Wide-Scope Screening Method for Multiclass Veterinary Drug Residues in Fish, Shrimp, and Eel Using Liquid Chromatography-Quadrupole High-Resolution Mass Spectrometry.

    Science.gov (United States)

    Turnipseed, Sherri B; Storey, Joseph M; Lohne, Jack J; Andersen, Wendy C; Burger, Robert; Johnson, Aaron S; Madson, Mark R

    2017-01-13

    A screening method for veterinary drug residues in fish, shrimp, and eel using LC with a high-resolution MS instrument has been developed and validated. The method was optimized for over 70 test compounds representing a variety of veterinary drug classes. Tissues were extracted by vortex mixing with acetonitrile acidified with 2% acetic acid and 0.2% p-toluenesulfonic acid. A centrifuged portion of the extract was passed through a novel solid phase extraction cartridge designed to remove interfering matrix components from tissue extracts. The eluent was then evaporated and reconstituted for analysis. Data were collected with a quadrupole-Orbitrap high-resolution mass spectrometer using both nontargeted and targeted acquisition methods. Residues were detected on the basis of the exact mass of the precursor and a product ion along with isotope pattern and retention time matching. Semiquantitative data analysis compared MS(1) signal to a one-point extracted matrix standard at a target testing level. The test compounds were detected and identified in salmon, tilapia, catfish, shrimp, and eel extracts fortified at the target testing levels. Fish dosed with selected analytes and aquaculture samples previously found to contain residues were also analyzed. The screening method can be expanded to monitor for an additional >260 veterinary drugs on the basis of exact mass measurements and retention times.

  14. Screening and identification of unknown contaminants in water with liquid chromatography and quadrupole-orthogonal acceleration-time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Bobeldijk, I; Vissers, J P; Kearney, G; Major, H; Van Leerdam, J A

    2001-09-21

    In order to assess and maintain the quality of surface waters, target compound monitoring is often not sufficient. Many unknown micro-contaminants are present in water, originating in municipal, industrial or agricultural effluents. Some of these might pose a risk to drinking water production and consequently to human health. The possibilities of screening surface water and identification of these non-target water pollutants with modern data acquisition possibilities of hybrid quadrupole-orthogonal acceleration time of flight mass spectrometers (Q-TOF), such as data-dependent MS to MS/MS switching were investigated. Using model compounds, a procedure for the liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening of water extracts was developed, enabling the detection and identification of compounds at levels < or = 0.25 microg/l in surface water. Based on the accurate mass the elemental compositions for the precursor and product ions are calculated. The calculated chemical formulae are searched against the Merck index, the NIST library, an own database containing about 2,500 water pollutants (pesticides and other contaminants) as well as a CI-CID library containing tandem MS spectra of about 100 water contaminants. The developed approach was applied for the identification of unknown compounds, present in native surface water extract. For three of these compounds, structures were proposed. Confirmation of the proposed structures with standards was beyond the scope of this study.

  15. Combining Fourier transform nuclear quadrupole resonance (FT-NQR) spectroscopy and mass spectrometry (MS) to study the electronic structure of titanocene dichlorides.

    Science.gov (United States)

    Kubišta, Jiří; Civiš, Martin; Spaněl, Patrik; Civiš, Svatopluk

    2012-03-21

    A combination of nuclear quadrupole resonance spectroscopy (NQR) and mass spectrometry (MS) has been used to observe trends in electronic structure in three titanocenes: bis(cyclopentadienyl) titanium dichloride (η(5)-C(5)H(5))(2)TiCl(2), bis(pentamethylcyclopentadienyl) titanium dichloride (η(5)-C(5)(CH(3))(5))(2)TiCl(2) and dimethylsilylene-bridged ansa bis(cyclopentadienyl) titanium dichloride Si(CH(3))(2)(η(5)-C(5)H(5))(2)TiCl(2). Using MS, electron ionisation mass spectra of these compounds are presented within the context of the entire homologous series with one to five methyl groups on each cyclopentadienyl ligand. A dedicated NQR spectrometer was constructed for this study with a sensitivity sufficient to precisely determine the NQR resonant frequency of (35)Cl atoms using 3 g samples of these titanocenes. The observed frequencies are thus 11.784, 11.930 and 10.863 MHz at 298 K. The results demonstrate that NQR using a relatively simple apparatus can be used as a sensitive and cost effective probe into the molecular structure of organometallic chlorides, which complements the information inferred from the mass spectra.

  16. A collinear tandem time-of-flight mass spectrometer for infrared photodissociation spectroscopy of mass-selected ions

    Institute of Scientific and Technical Information of China (English)

    WANG GuanJun; CHI ChaoXian; XING XiaoPeng; DING ChuanFan; ZHOU MingFei

    2014-01-01

    An apparatus based on collinear tandem time-of-flight mass spectrometer has been designed for the measurement of infrared photodissociation spectroscopy of mass-selected ions in the gas phase.The ions from a pulsed laser vaporization supersonic ion source are skimmed and mass separated by a Wiley-McLaren time-of-flight mass spectrometer.The ion of interest is mass selected,decelerated and dissociated by a tunable IR laser.The fragment and parent ions are reaccelerated and mass analyzed by the second time-of-flight mass spectrometer.A simple new assembly integrated with mass gate,deceleration and reacceleration ion optics was designed,which allows us to measure the infrared spectra of mass selected ions with high sensitivity and easy timing synchronization.

  17. Multiresidue analysis of plant growth regulators in grapes by triple quadrupole and quadrupole-time of flight-based liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Oulkar, Dasharath P; Banerjee, Kaushik; Kulkarni, Sunil

    2011-01-01

    A selective and sensitive LC-MS/MS method is presented for simultaneous determination of 12 plant growth regulators, viz., indol-3-acetic acid, indol-3-butyric acid, kinetin, zeatin, 6-benzyl aminopurine, gibberellic acid, abscisic acid, chlormequat chloride, forchlorfenuron, paclobutrazole, daminozide, and 2,4-dichlorophenoxy acetic acid, in bud sprouts and grape berries. The sample preparation method involved extraction of homogenized sample (5 g) with 40 mL methanol (80%), and final determination was by LC-MS/MS in the multiple reaction monitoring (MRM) mode with time segmentation for quantification supported by complementary analysis by quadrupole-time of flight (Q-TOF) MS with targeted high-resolution MS/MS scanning for confirmatory identification based on accurate mass measurements. The recovery of the test compounds ranged within 90-107% with precision RSD less than 5% (n = 6). The method could be successfully applied in analyzing incurred residue samples, and the strength of accurate mass analysis could be utilized in identifying the compounds in cases where the qualifier MRM ions were absent or at an S/N less than 3:1 due to low concentrations.

  18. A Micro Cylindrical Ion Trap (5-CIT) Micro Mass Spectrometer Instrument System (5MSIS) for NASA Planetary Exploration Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The project aims to develop a miniature packaging platform for the integration of MEMS mass spectrometer components to form the basis of a Micro Mass Spectrometer...

  19. Simultaneous determination of iridoid glycosides, phenethylalcohol glycosides and furfural derivatives in Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass spectrometry

    DEFF Research Database (Denmark)

    Xu, Jun; Wu, Jie; Zhu, Ling-Ying

    2012-01-01

    In this study, a sensitive and selective method for simultaneously quantifying eight major components (four iridoid glycosides, three phenethylalcohol glycosides and one furfural derivative) of Rehmanniae Radix by high performance liquid chromatography coupled with triple-quadrupole mass...

  20. Gas chromatography–triple quadrupole mass spectrometry for the determination of atmospheric polychlorinated naphthalenes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Fang [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Jin, Jing [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Sun, Xiaoli [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Wang, Xueli; Li, Yun; Shah, Syed Mazhar [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China)

    2014-09-15

    Highlights: • Atmospheric PCNs were detected by isotope-dilution GC–MS/MS. • The pollution levels of PCNs covering from mono- to octa-CNs were investigated comprehensively in air samples. • The dioxin-like toxicity and human exposure levels of PCNs in air samples were estimated. - Abstract: Atmospheric polychlorinated naphthalenes (PCNs) ranging from mono-CNs to octa-CNs were detected using isotope-dilution gas chromatography coupled with triple quadrupole mass spectrometry (GC–MS/MS). The developed instrumental method was successfully applied to the determination of PCNs in technical products. It was observed that there were significant differences in concentrations, homologue profiles, chlorinated contents and total toxic equivalents (∑TEQs) of PCNs for four Halowax products. Subsequently, the validation of the analytical method was evaluated for the determination of PCNs in air samples in terms of method detection limit (MDL), recovery and matrix effect. The results demonstrated that this method could provide satisfactory sensitivity and adequate selectivity with lower cost. It was conducted to comprehensively evaluate the levels, composition patterns, ∑TEQs, and daily intake exposure of PCNs in indoor and outdoor air samples. Concentrations and ∑TEQs of PCNs in air samples ranged 47.7–832.7 pg m{sup −3} and 1.31–5.99 fg m{sup −3}, respectively, and the predominant homologues were di- and tri-CNs in the gas phase. The results indicated that this analytical method was useful for the accurate and specific evaluation of dioxin-like toxicity and human exposure levels of PCNs in the atmosphere.

  1. Analysis of butadiene urinary metabolites by liquid chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    McDonald, Jacob D; Bechtold, William E; Krone, Jennifer R; Blackwell, Walter B; Kracko, Dean A; Henderson, Rogene F

    2004-04-01

    1,3-Butadiene (BD) is a monomer produced in petrochemical production facilities and from several combustion sources. The United States Environmental Protection Agency has defined BD as a probable human carcinogen. Methods for assessing exposure and internal dose are therefore of critical interest, and one technique is the measurement of urinary metabolites. Here we describe methods for measuring two urinary metabolites, N-acetyl-S-(3,4-dihydroxybutyl)-L-cysteine (referred to as MI) and an isomeric mixture of the regio- and stereoisomers (R)/(S)-N-acetyl-S-(1-(hydroxymethyl)-2-propen-yl)-L-cysteine and (R)/(S)-N-acetyl-S-(2-hydroxy-3-butenyl)-L-cysteine (referred to as MII). The method is based on isolation of the metabolites by solid-phase extraction and measurement using liquid chromatography and triple quadrupole mass spectrometry (LC-MS(3)). The LC-MS(3) allowed good selectivity with minimal sample preparation. Assay accuracy was within 10% or better, with substantial improvement in accuracy accompanying the commercial availability of deuterated internal standards for both compounds. Assay precision and linearity passed rigorous validation criteria, and precision-based limits of quantitation values were 12 and 1 ng/mL for MI and MII, respectively. Data are shown from analysis of human urine from occupationally exposed individuals and rat urine from BD exposures conducted to investigate rodent metabolic profiles. Both of these data sets clearly show that this assay can discern previously described relationships between BD exposure and the production of MI/MII.

  2. SIEMENS ADVANCED QUANTRA FTICR MASS SPECTROMETER FOR ULTRA HIGH RESOLUTION AT LOW MASS

    Energy Technology Data Exchange (ETDEWEB)

    Spencer, W; Laura Tovo, L

    2008-07-08

    The Siemens Advanced Quantra Fourier Transform Ion Cyclotron Resonance (FTICR) mass spectrometer was evaluated as an alternative instrument to large double focusing mass spectrometers for gas analysis. High resolution mass spectrometers capable of resolving the common mass isomers of the hydrogen isotopes are used to provide data for accurate loading of reservoirs and to monitor separation of tritium, deuterium, and helium. Conventional double focusing magnetic sector instruments have a resolution that is limited to about 5000. The Siemens FTICR instrument achieves resolution beyond 400,000 and could possibly resolve the tritium ion from the helium-3 ion, which differ by the weight of an electron, 0.00549 amu. Working with Y-12 and LANL, SRNL requested Siemens to modify their commercial Quantra system for low mass analysis. To achieve the required performance, Siemens had to increase the available waveform operating frequency from 5 MHz to 40 MHz and completely redesign the control electronics and software. However, they were able to use the previous ion trap, magnet, passive pump, and piezo-electric pulsed inlet valve design. NNSA invested $1M in this project and acquired four systems, two for Y-12 and one each for SRNL and LANL. Siemens claimed a $10M investment in the Quantra systems. The new Siemens Advanced Quantra demonstrated phenomenal resolution in the low mass range. Resolution greater than 400,000 was achieved for mass 2. The new spectrometer had a useful working mass range to 500 Daltons. However, experiments found that a continuous single scan from low mass to high was not possible. Two useful working ranges were established covering masses 1 to 6 and masses 12 to 500 for our studies. A compromise performance condition enabled masses 1 to 45 to be surveyed. The instrument was found to have a dynamic range of about three orders of magnitude and quantitative analysis is expected to be limited to around 5 percent without using complex fitting algorithms

  3. Note: A versatile mass spectrometer chamber for molecular beam and temperature programmed desorption experiments

    Science.gov (United States)

    Tonks, James P.; Galloway, Ewan C.; King, Martin O.; Kerherve, Gwilherm; Watts, John F.

    2016-08-01

    A dual purpose mass spectrometer chamber capable of performing molecular beam scattering (MBS) and temperature programmed desorption (TPD) is detailed. Two simple features of this design allow it to perform these techniques. First, the diameter of entrance aperture to the mass spectrometer can be varied to maximize signal for TPD or to maximize angular resolution for MBS. Second, the mass spectrometer chamber can be radially translated so that it can be positioned close to the sample to maximize signal or far from the sample to maximize angular resolution. The performance of this system is described and compares well with systems designed for only one of these techniques.

  4. Note: A versatile mass spectrometer chamber for molecular beam and temperature programmed desorption experiments

    Energy Technology Data Exchange (ETDEWEB)

    Tonks, James P., E-mail: james.tonks@awe.co.uk [Department of Mechanical Engineering Sciences, University of Surrey, Guildford, Surrey GU2 7XH (United Kingdom); AWE Plc, Aldermaston, Reading, Berkshire RG7 4PR (United Kingdom); Galloway, Ewan C., E-mail: ewan.galloway@awe.co.uk; King, Martin O. [AWE Plc, Aldermaston, Reading, Berkshire RG7 4PR (United Kingdom); Kerherve, Gwilherm [VACGEN Ltd, St. Leonards-On-Sea, East Sussex TN38 9NN (United Kingdom); Watts, John F. [Department of Mechanical Engineering Sciences, University of Surrey, Guildford, Surrey GU2 7XH (United Kingdom)

    2016-08-15

    A dual purpose mass spectrometer chamber capable of performing molecular beam scattering (MBS) and temperature programmed desorption (TPD) is detailed. Two simple features of this design allow it to perform these techniques. First, the diameter of entrance aperture to the mass spectrometer can be varied to maximize signal for TPD or to maximize angular resolution for MBS. Second, the mass spectrometer chamber can be radially translated so that it can be positioned close to the sample to maximize signal or far from the sample to maximize angular resolution. The performance of this system is described and compares well with systems designed for only one of these techniques.

  5. Wavelet-based method for time-domain noise analysis and reduction in a frequency-scan ion trap mass spectrometer.

    Science.gov (United States)

    Chou, Szu-Wei; Shiu, Guo-Rung; Chang, Huan-Cheng; Peng, Wen-Ping

    2012-11-01

    We adopt an orthogonal wavelet packet decomposition (OWPD) filtering approach to cancel harmonic interference noises arising from an AC power source in time domain and remove the resulting rf voltage interference noise from the mass spectra acquired by using a charge detection frequency-scan quadrupole ion trap mass spectrometer. With the use of a phase lock resampling technique, the transform coefficients of the rf interference in signals become a constant, exhibiting a shift of the baseline in different rf phases. The rf interference is therefore removable by shifting the baselines back to zero in OWPD coefficients. The approach successfully reduces the time-domain background noise from 1367 electrons (rms) to 408 electrons (rms) (an improvement of 70 %) and removes the high frequency noise components in the charge detection ion trap mass spectrometry. Unlike other smoothing or averaging methods commonly used in the mass-to-charge (m/Ze) domain, our approach does not cause any distortion of original signals.

  6. Large Acceptance Spectrometers for Invariant Mass Spectroscopy of Exotic Nuclei and Future Development

    CERN Document Server

    Nakamura, T

    2015-01-01

    Large acceptance spectrometers at in-flight RI separators have played significant roles in investigating the structure of exotic nuclei. Such spectrometers are in particular useful for probing unbound states of exotic nuclei, using invariant mass spectroscopy with reactions at intermediate and high energies. We discuss here the key characteristic features of such spectrometers, by introducing the recently commissioned SAMURAI facility at the RIBF, RIKEN. We also explore the issue of cross talk in the detection of multiple neutrons, which has become crucial for exploring further unbound states and nuclei beyond the neutron drip line. Finally we discuss future perspectives for large acceptance spectrometers at the new-generation RI-beam facilities.

  7. Large acceptance spectrometers for invariant mass spectroscopy of exotic nuclei and future developments

    Energy Technology Data Exchange (ETDEWEB)

    Nakamura, T.; Kondo, Y.

    2016-06-01

    Large acceptance spectrometers at in-flight RI separators have played significant roles in investigating the structure of exotic nuclei. Such spectrometers are in particular useful for probing unbound states of exotic nuclei, using invariant mass spectroscopy with reactions at intermediate and high energies. We discuss here the key characteristic features of such spectrometers, by introducing the recently commissioned SAMURAI facility at the RIBF, RIKEN. We also investigate the issue of cross talk in the detection of multiple neutrons, which has become crucial for exploring further unbound states and nuclei beyond the neutron drip line. Finally we discuss future perspectives for large acceptance spectrometers at the new-generation RI-beam facilities.

  8. A targeted/non-targeted screening method for perfluoroalkyl carboxylic acids and sulfonates in whole fish using quadrupole time-of-flight mass spectrometry and MS(e).

    Science.gov (United States)

    Crimmins, Bernard S; Xia, Xiaoyan; Hopke, Philip K; Holsen, Thomas M

    2014-02-01

    A new method for measuring perfluoroalkyl contaminants (PFCs) in biological matrices has been developed. An ultra-high pressure liquid chromatograph equipped with a quadrupole time-of-flight mass spectrometer (UPLC-QToF) was optimized using a continuous precursor/product ion monitoring mode. Unlike traditional targeted studies that isolate precursor/product ion pairs, the current method alternates between two ionization energy channels to continuously capture standard electrospray ionization (low energy) and collision induced dissociation (high energy) spectra. The result is the indiscriminant acquisition of paired low and high energy spectra for all constituents eluting from the chromatographic system. This technique was evaluated for the routine analysis of perfluoroalkyl species. Using this technique, linear perfluoroalkyl carboxylic acids (C4 to C14) and perfluoroalkyl sulfonates (C4, C6, C8 and C10) exhibited a linear range spanning over three orders of magnitude and were detectable at levels less than 1 pg on column with a root mean squared signal to noise ratio of 5 to 20. Lake trout (Salvelinus namaycush) and National Institutes of Standards and Technology Standard Reference Material 1946 were used to evaluate matrix effects and the accuracy of this method when applied to a whole fish extract. The current method was also evaluated as a diagnostic tool to identify unknown PFCs using experimental fragmentation patterns, mass defect filtering and Kendrick plots.

  9. Standard test method for analysis of isotopic composition of uranium in nuclear-grade fuel material by quadrupole inductively coupled plasma-mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method is applicable to the determination of the isotopic composition of uranium (U) in nuclear-grade fuel material. The following isotopic weight percentages are determined using a quadrupole inductively coupled plasma-mass spectrometer (Q-ICP-MS): 233U, 234U, 235U, 236U, and 238U. The analysis can be performed on various material matrices after acid dissolution and sample dilution into water or dilute nitric (HNO3) acid. These materials include: fuel product, uranium oxide, uranium oxide alloys, uranyl nitrate (UNH) crystals, and solutions. The sample preparation discussed in this test method focuses on fuel product material but may be used for uranium oxide or a uranium oxide alloy. Other preparation techniques may be used and some references are given. Purification of the uranium by anion-exchange extraction is not required for this test method, as it is required by other test methods such as radiochemistry and thermal ionization mass spectroscopy (TIMS). This test method is also described i...

  10. Miniature Time of Flight Mass Spectrometer for Space and Extraterrestrial Applications Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The PI has developed a miniature time-of-flight mass spectrometer (TOF-MS), which can be op-timized for space and extraterrestrial applications, by using a...

  11. Development and Deployment of Retrofit PolarisQ Ion Trap Mass Spectrometer for Isotope Ratio Measurements

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Cyril V. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Whitten, William B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2015-11-01

    This report describes Oak Ridge National Laboratory’s (ORNL) FY15 progress in support of National Nuclear Security Administration’s (NNSA) Portable Mass Spectrometer project. A retrofit PolarisQ ion trap mass spectrometer (RPMS) has been assembled from components of two PolarisQ ion trap mass spectrometers used in previous isotope ratio programs. The retrofit mass spectrometer includes a custom Hastelloy vacuum chamber which is about ¼ the size of the standard aluminum vacuum chamber and reduces the instrument weight from the original by nine pounds. In addition, the new vacuum chamber can be independently heated to reduce impurities such as water, which reacts with UF6 to produce HF in the vacuum chamber. The analyzer and all components requiring service are mounted on the chamber lid, facilitating quick and easy replacement of consumable components such as the filament and electron multiplier.

  12. Optimization of the isotopic analysis of UF{sub 6} by quadrupole mass spectrometry technique; Otimizacao da analise isotopica de UF{sub 6} utilizando-se a tecnica de espectrometria de massas por quadrupolo

    Energy Technology Data Exchange (ETDEWEB)

    Porto, Peterson

    2006-07-01

    In the present work a procedure for determination of the isotopic ratio {sup 238}U/{sup 235}U in UF{sub 6} samples was established using a quadrupole mass spectrometer with ionization by electron impact and ion detection by Faraday cup or electron multiplier. For this, the following items were optimized in the spectrometer: the parameters in the ion source that provided the most intense peak, with good shape, for the corresponding mass of the most abundant isotope; the resolution that reduced the non linear effects and the number of analytic cycles that reduced the uncertainty in the results. The measurement process was characterized with respect to the effects of mass discrimination, linearity and memory effect. The mass discrimination showed to be linearly dependent of the sample pressure in the batch volume, for the pressure ranges from 0.15 to 0.30 mbar and from 0.30 to 0.40 mbar. The spectrometer was shown linear in the measurement of isotopic ratios between 0.005 and 0.045. The memory factor for the ion source and for the introduction system were, respectively, 1.000 {+-} 0.001 and 1.003 {+-} 0.003; the first one can be ignored, the second one can be eliminated by washing the batch volume with the new sample. A methodology for routine analysis of UF{sub 6} samples and the determination of the uncertainties were set up in details as well. (author)

  13. Continuation of Mass determinations through a Double Focusing Mass Spectrometer on Line with ISOLDE

    CERN Multimedia

    2002-01-01

    In a previous experiment (1976-77) we have demonstrated the interest and feasibility of atomic mass determinations from the direct measurements of mass ratios on Rb, Cs and Fr isotopes. Masses of long series of isotopes on both side of stability were determined with an accuracy of a few tens to 300 keV (for th exotic). Interesting nuclear structure features could be observed as for example the indication for an onset of deformation, at N~=~60 for Z~=~37, which stimulated further experiments and theoretical calculations. The many mass values, until then unknown, we obtained in our experiments, gave in addition the possibility to make detailed tests of the nuclear mass predictions. Due to improvements on our mass spectrometer (better transmission and higher resolving power) and increased ISOLDE production yields, some new and valuable measurements can be performed. We plan: \\item a) to continue the measurements towards even heavier isotopes and explore the deformation regions which start at |9|7Rb and |1|4|6Cs;...

  14. Rapid screening and identification of lycodine-type alkaloids in Lycopodiaceae and Huperziaceae plants by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Shan, Si-Ming; Luo, Jian-Guang; Pan, Ke; Zou, Hong-Yan; Kong, Ling-Yi

    2016-11-01

    Lycodine-type alkaloids have gained significant interest owing to their unique skeletal characteristics and acetylcholinesterase activity. This study established a rapid and reliable method using ultra-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-ESI-Q/TOF-MS/MS) for comprehensive characterization of lycodine-type alkaloids for the first time. The lycodine-type alkaloids were detected successfully from Lycopodiastrum casuarinoides, Huperzia serrata and Phlegmarirus carinatus in seven plants of the Lycopodiaceae and Huperziaceae families, based on the established characteristic MS fragmentation of five known alkaloids. Furthermore, a total of 13 lycodine-type alkaloids were identified, of which three pairs of isomers were structurally characterized and differentiated. This study further improves mass analysis of lycodine-type alkaloids and demonstrates the superiority of UPLC with a high-resolution mass spectrometer for the rapid and sensitive structural elucidation of other trace active compounds. Copyright © 2016 John Wiley & Sons, Ltd.

  15. Mobility Peak Tailing Reduction in a Differential Mobility Analyzer (DMA) Coupled with a Mass Spectrometer and Several Ionization Sources

    Science.gov (United States)

    Amo-Gonzalez, Mario; Fernandez de la Mora, Juan

    2017-08-01

    The differential mobility analyzer (DMA) is a narrow-band linear ion mobility filter operating at atmospheric pressure. It combines in series with a quadrupole mass spectrometer (Q-MS) for mobility/mass analysis, greatly reducing chemical noise in selected ion monitoring. However, the large flow rate of drift gas ( 1000 L/min) required by DMAs complicates the achievement of high gas purity. Additionally, the symmetry of the drying counterflow gas at the interface of many commercial MS instruments, is degraded by the lateral motion of the drift gas at the DMA entrance slit. As a result, DMA mobility peaks often exhibit tails due to the attachment of impurity vapors, either (1) to the reagent ion within the separation cell, or (2) to the analyte of interest in the ionization region. In order to greatly increase the noise-suppression capacity of the DMA, we describe various vapor-removal schemes and measure the resulting increase in the tailing ratio, ( TR = signal at the peak maximum over signal two half-widths away from this maximum). Here we develop a low-outgassing DMA circuit connected to a mass spectrometer, and test it with three ionization sources (APCI, Desolvating-nano ESI, and Desolvating low flow SESI). While prior TR values were in the range 100-1000, the three new sources achieve TR 105. The SESI source has been optimized for maximum sensitivity, delivering an unprecedented gain for TNT of 190 counts/fg, equivalent to an ionization efficiency of one out of 140 neutral molecules.

  16. Molecular beam mass spectrometer equipped with a catalytic wall reactor for in situ studies in high temperature catalysis research

    Science.gov (United States)

    Horn, R.; Ihmann, K.; Ihmann, J.; Jentoft, F. C.; Geske, M.; Taha, A.; Pelzer, K.; Schlögl, R.

    2006-05-01

    A newly developed apparatus combining a molecular beam mass spectrometer and a catalytic wall reactor is described. The setup has been developed for in situ studies of high temperature catalytic reactions (>1000°C), which involve besides surface reactions also gas phase reactions in their mechanism. The goal is to identify gas phase radicals by threshold ionization. A tubular reactor, made from the catalytic material, is positioned in a vacuum chamber. Expansion of the gas through a 100μm sampling orifice in the reactor wall into differentially pumped nozzle, skimmer, and collimator chambers leads to the formation of a molecular beam. A quadrupole mass spectrometer with electron impact ion source designed for molecular beam inlet and threshold ionization measurements is used as the analyzer. The sampling time from nozzle to detector is estimated to be less than 10ms. A detection time resolution of up to 20ms can be reached. The temperature of the reactor is measured by pyrometry. Besides a detailed description of the setup components and the physical background of the method, this article presents measurements showing the performance of the apparatus. After deriving the shape and width of the energy spread of the ionizing electrons from measurements on N2 and He we estimated the detection limit in threshold ionization measurements using binary mixtures of CO in N2 to be in the range of several hundreds of ppm. Mass spectra and threshold ionization measurements recorded during catalytic partial oxidation of methane at 1250°C on a Pt catalyst are presented. The detection of CH3• radicals is successfully demonstrated.

  17. Wide-scope screening and quantification of 50 pesticides in wine by liquid chromatography/quadrupole time-of-flight mass spectrometry combined with liquid chromatography/quadrupole linear ion trap mass spectrometry.

    Science.gov (United States)

    He, Zeying; Xu, Yaping; Wang, Lu; Peng, Yi; Luo, Ming; Cheng, Haiyan; Liu, Xiaowei

    2016-04-01

    In this paper, a wide scope screening method of pesticides in wine was established using liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QTOF MS) and liquid chromatography/quadrupole linear ion trap mass spectrometry (LC-QqLIT MS). Information dependent acquisition (IDA) experiments are used to obtain both MS and MS/MS information for LC-QTOF MS analysis. For LC-QqLIT MS analysis, MS/MS spectra of target pesticides were simultaneously acquired using Enhanced Product Ion (EPI) mode at very low concentrations to increase the confidence in analytical results of multiple reaction monitoring (MRM) by library searching. Method validation was carried out using 50 pesticides commonly used in vineyards. The LOQs, linearity, repeatability were determined and good enough for quantification. The screening and quantification results obtained using LC-QTOF MS and LC-QqLIT MS were compared. Contaminants were screened against libraries containing over 2800 compounds based on accurate mass, isotopic patterns, and MS/MS spectra searching to extend the scope of this methodology to non-target screening.

  18. A compact E × B filter: A multi-collector cycloidal focusing mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Blase, Ryan C., E-mail: rblase@swri.edu; Miller, Greg; Brockwell, Tim; Waite, J. Hunter [Southwest Research Institute, 6220 Culebra Road, San Antonio, Texas 78238 (United States); Westlake, Joseph [The Johns Hopkins University Applied Physics Laboratory LLC, 11100 Johns Hopkins Road, Laurel, Maryland 20723 (United States); Ostrom, Nathaniel; Ostrom, Peggy H. [Department of Integrative Biology, Michigan State University, 288 Farm Lane RM 203, East Lansing, Michigan 48824 (United States)

    2015-10-15

    A compact E × B mass spectrometer is presented. The mass spectrometer presented is termed a “perfect focus” mass spectrometer as the resolution of the device is independent of both the initial direction and energy of the ions (spatial and energy independent). The mass spectrometer is small in size (∼10.7 in.{sup 3}) and weight (∼2 kg), making it an attractive candidate for portability when using small, permanent magnets. A multi-collector Faraday cup design allows for the detection of multiple ion beams in discrete collectors simultaneously; providing the opportunity for isotope ratio monitoring. The mass resolution of the device is around 400 through narrow collector slits and the sensitivity of the device follows expected theoretical calculations of the ion current produced in the electron impact ion source. Example mass spectra obtained from the cycloidal focusing mass spectrometer are presented as well as information on mass discrimination based on instrumental parameters and isotope ratio monitoring of certain ion signals in separate Faraday cups.

  19. First direct mass measurements on nobelium and lawrencium with the Penning trap mass spectrometer SHIPTRAP

    Energy Technology Data Exchange (ETDEWEB)

    Dworschak, Michael Gerhard

    2009-12-08

    The Penning trap mass spectrometer SHIPTRAP at GSI Darmstadt was set up for high-precision mass measurements of heavy radionuclides produced in fusion evaporation reactions and separated from the primary beam by the velocity filter SHIP. It consists of a gas stopping cell for the deceleration of the high energetic reaction products, an RFQ cooler and buncher for cooling and accumulation of the ions, and a double Penning trap system to perform mass measurements. The mass is determined by measuring the cyclotron frequency of the ion of interest in a strong homogeneous magnetic field and comparing it to the frequency of a well-known reference ion. With this method relative uncertainties in the order of 10{sup -8} can be achieved. Recently, mass measurements of the three nobelium isotopes {sup 252-254}No (Z=102) and the lawrencium isotope {sup 255}Lr (Z=103) were performed successfully. These were the first direct mass measurements of transuranium elements ever per- formed. The production rate of the atoms of interest was about one per second or less. The results of the measurements on nobelium confirm the previous mass values which were deduced from Q{sub {alpha}} values. In the case of {sup 255}Lr the mass excess value, which was previously only estimated from systematic trends, was for the first time directly measured. These results mark the first step in the exploration of the region of transuranium elements which is planned at SHIPTRAP. The main objective is to fix the endpoints of {alpha} decay chains which are originating from superheavy elements close to the predicted island of stability. (orig.)

  20. Targeted analysis with benchtop quadrupole–orbitrap hybrid mass spectrometer: Application to determination of synthetic hormones in animal urine

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Praveen [Departament de Química Analítica, Universitat de Barcelona, Barcelona (Spain); Rúbies, Antoni; Centrich, Francesc [Laboratori Agència Salut Pública de Barcelona, Barcelona (Spain); CIBER of Epidemiology and Public Health (CIBERESP), Madrid (Spain); Granados, Mercè [Departament de Química Analítica, Universitat de Barcelona, Barcelona (Spain); Cortés-Francisco, Nuria; Caixach, Josep [Mass Spectrometry Laboratory-Organic Pollutants, IDAEA-CSIC, Barcelona (Spain); Companyó, Ramon, E-mail: compano@ub.edu [Departament de Química Analítica, Universitat de Barcelona, Barcelona (Spain)

    2013-05-30

    Graphical abstract: -- Highlights: •The quadrupole in Q Exactive acts as a powerful filter to reduce ion suppression. •Reducing mass range using quadrupole in targeted modes increases the S/N ratio. •Targeted SIM data dependent scan modes are the most suitable for residue analysis. •A HRMS confirmatory method for synthetic hormones in urine has been developed. •The Q Exactive provides similar sensitivity and enhanced selectivity compared to QqQ. -- Abstract: Sensitive and unequivocal determination of analytes/contaminants in complex matrices is a challenge in the field of food safety control. In this study, various acquisition modes (Full MS/AIF, Full MS + tMS/MS, Full MS/dd MS/MS and tSIM/ddMS/MS) and parameters of a quadrupole–orbitrap hybrid mass spectrometer (Q Exactive) were studied in detail. One of the main conclusions has been that, reducing the scan range for Full MS (using the quadrupole) and targeted modes give higher signal-to-noise (S/N) ratios and thereby better detection limits for analytes in matrix. The use of Q Exactive in a complex case, for the confirmatory analysis of hormones in animal urine is presented. A targeted SIM data dependent MS/MS (tSIM/ddMS/MS) acquisition method for determination of eight synthetic hormones (trenbolone, 17α ethinylestradiol, zeranol, stanozolol, dienestrol, diethylstilbestrol, hexestrol, taleranol) and a naturally occurring hormone (zearalenone) in animal urine were optimized to have sensitive precursors from targeted SIM mode and trigger MS/MS scans over the entire chromatograph peak. The method was validated according to EC/657/2002. CCα (decision limit) for the analytes ranged between 0.11 μg L{sup −1} and 0.69 μg L{sup −1} and CCβ (detection capability) ranged between 0.29 μg L{sup −1} and 0.90 μg L{sup −1}.

  1. Direct analysis of pharmaceutical drug formulations using ion mobility spectrometry/quadrupole-time-of-flight mass spectrometry combined with desorption electrospray ionization.

    Science.gov (United States)

    Weston, Daniel J; Bateman, Robert; Wilson, Ian D; Wood, Tim R; Creaser, Colin S

    2005-12-01

    A novel approach to the rapid analysis of pharmaceutical drug formulations using hyphenated ion mobility spectrometry (IMS) and time-of-flight mass spectrometry (ToF-MS) that requires no sample pretreatment or chromatographic separation is described. A modified quadrupole time-of-flight mass spectrometer containing an ion mobility drift cell was used for gas-phase electrophoretic separation of ions prior to ToF-MS detection. The generation of sample ions directly from tablets and cream formulations was effected by desorption electrospray ionization (DESI) using a modified electrospray ion source. The analysis of a range of over-the-counter and prescription tablet formulations is described, including histamine H2 receptor antagonist (ranitidine), analgesic (paracetamol), opiate (codeine), and aromatase inhibitor anticancer (anastrozole) drugs. The successful determination of active drugs from soft formulations, such as an antiseptic cream (chlorhexidine) and a nicotine-containing skin patch, is also presented. Limits of detection for the active drugs using the DESI/IMS/ToF-MS method fell within the high-picomole to nanomole range. In all cases, the use of ion mobility drift tube separation showed increased selectivity for active drug responses (present as low as 0.14% w/w) over excipient responses such as poly(ethylene glycol). Tandem mass spectrometric analysis of precursor ions separated by IMS allowed positive confirmation of active drugs with little loss of ion mobility efficiency. The ability to analyze hard or soft pharmaceutical formulations directly by DESI combined with ion mobility spectrometry/mass spectrometry in approximately 2 min demonstrates the potential applicability of this novel method to pharmaceutical screening of low-molecular-weight drug formulations with high selectivity over the formulation vehicle.

  2. Modified quadrupole mass analyzer RGA-100 for beam plasma research in forevacuum pressure range

    Energy Technology Data Exchange (ETDEWEB)

    Zolotukhin, D. B.; Tyunkov, A. V. [Tomsk State University of Control Systems and Radioelectronics, 40 Lenin Ave., Tomsk 634050 (Russian Federation); Yushkov, Yu. G., E-mail: yuyushkov@gmail.com [Tomsk State University of Control Systems and Radioelectronics, 40 Lenin Ave., Tomsk 634050 (Russian Federation); Tomsk Polytechnic University, 30 Lenin Ave., Tomsk 634050 (Russian Federation); Oks, E. M. [Tomsk State University of Control Systems and Radioelectronics, 40 Lenin Ave., Tomsk 634050 (Russian Federation); Institute of High Current Electronics SB RAS, 2/3, Akademichesky Ave., Tomsk 634055 (Russian Federation)

    2015-12-15

    The industrial quadrupole RGA-100 residual gas analyzer was modified for the research of electron beam-generated plasma at forevacuum pressure range. The standard ionizer of the RGA-100 was replaced by three electrode extracting unit. We made the optimization of operation parameters in order to provide the maximum values of measured currents of any ion species. The modified analyzer was successfully tested with beam plasma of argon, nitrogen, oxygen, and hydrocarbons.

  3. Trace analysis of pesticides in paddy field water by direct injection using liquid chromatography-quadrupole-linear ion trap-mass spectrometry.

    Science.gov (United States)

    Pareja, Lucía; Martínez-Bueno, M J; Cesio, Verónica; Heinzen, Horacio; Fernández-Alba, A R

    2011-07-29

    A multiresidue method was developed for the quantification and confirmation of 70 pesticides in paddy field water. After its filtration, water was injected directly in a liquid chromatograph coupled to a hybrid triple quadrupole-linear ion trap-mass spectrometer (QqLIT). The list of target analytes included organophosphates, phenylureas, sulfonylureas, carbamates, conazoles, imidazolinones and others compounds widely used in different countries where rice is cropped. Detection and quantification limits achieved were in the range from 0.4 to 80 ng L(-1) and from 2 to 150 ng L(-1), respectively. Correlation coefficients for the calibration curves in the range 0.1-50 μg L(-1) were higher than 0.99 except for diazinon (0.1-25 μg L(-1)). Only 9 pesticides presented more than 20% of signal suppression/enhancement, no matrix effect was observed in the studied conditions for the rest of the target pesticides. The method developed was used to investigate the occurrence of pesticides in 59 water samples collected in paddy fields located in Spain and Uruguay. The study shows the presence of bensulfuron methyl, tricyclazole, carbendazim, imidacloprid, tebuconazole and quinclorac in a concentration range from 0.08 to 7.20 μg L(-1). Copyright © 2011 Elsevier B.V. All rights reserved.

  4. The application of headspace gas chromatography coupled to tandem quadrupole mass spectrometry for the analysis of furan in baby food samples.

    Science.gov (United States)

    Pugajeva, Iveta; Rozentale, Irina; Viksna, Arturs; Bartkiene, Elena; Bartkevics, Vadims

    2016-12-01

    Selective methodology employing a tandem quadrupole mass spectrometer coupled to a gas chromatograph with headspace autosampler (HS-GC-MS/MS) was elaborated in this study. Application of the elaborated procedure resulted in a limit of detection of 0.021μgkg(-1) and a limit of quantification of 0.071μgkg(-1). The mean recoveries during in-house validation ranged from 89% to 109%, and coefficients of variation for repeatability ranged from 4% to 11%. The proposed analytical method was applied for monitoring the furan content of 30 commercial baby food samples available on the Latvian retail market. The level of furan found in these samples varied from 0.45 to 81.9μgkg(-1), indicating that infants whose sole diet comprises baby food sold in jars and cans are exposed constantly to furan. Samples containing vegetables and meat had higher levels of furan than those containing only fruits. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Sources and atmospheric processing of organic aerosol in the Mediterranean: insights from aerosol mass spectrometer factor analysis

    Directory of Open Access Journals (Sweden)

    L. Hildebrandt

    2011-12-01

    Full Text Available Atmospheric particles were measured in the late winter (25 February–26 March 2009 at a remote coastal site on the island of Crete, Greece during the Finokalia Aerosol Measurement Experiment-2009. A quadrupole aerosol mass spectrometer (Q-AMS was employed to quantify the size-resolved chemical composition of non-refractory submicron aerosol, and a thermodenuder was used to analyze the organic aerosol (OA volatility. Complementary measurements included particle size distributions from a scanning mobility particle sizer, inorganic and organic particle composition from filter analysis, air ion concentrations, O3, NOx and NOy concentrations, and meteorological measurements. Factor analysis was performed on the OA mass spectra, and the variability in OA composition could best be explained with three OA components. The oxygenated organic aerosol (OOA was similar in composition and volatility to the summertime OA previously measured at this site and may represent an effective endpoint in particle-phase oxidation of organics. The two other OA components, one associated with amines (Amine-OA and the other probably associated with the burning of olive branches (OB-OA, had very low volatility but were less oxygenated. Hydrocarbon-like organic aerosol (HOA was not detected. The absence of OB-OA and Amine-OA in the summer data may be due to lower emissions and/or photochemical conversion of these components to OOA.

  6. Sources and atmospheric processing of organic aerosol in the Mediterranean: insights from aerosol mass spectrometer factor analysis

    Directory of Open Access Journals (Sweden)

    L. Hildebrandt

    2011-07-01

    Full Text Available Atmospheric particles were measured in the winter at a remote coastal site on the island of Crete, Greece during the Finokalia Aerosol Measurement Experiment-2009. A Quadrupole aerosol mass spectrometer (Q-AMS was employed to quantify the size-resolved chemical composition of non-refractory submicron aerosol, and a thermodenuder was used to analyze the organic aerosol (OA volatility. Complementary measurements included particle size distributions from a scanning mobility particle sizer, inorganic and organic particle composition from filter analysis, concentrations of O3, NOx and NOy, and meteorological measurements. Factor analysis was performed on the OA mass spectra, and the variability in OA composition could best be explained with three OA components. The oxygenated organic aerosol (OOA was similar in composition and volatility to the summertime OA previously measured at this site and appears to represent an effective endpoint in particle-phase oxidation of organics. The two other OA components, one associated with amines (Amine-OA and the other probably associated with the burning of olive branches (OB-OA, had lower volatility but were less oxygenated. Hydrocarbon-like organic aerosol (HOA was not detected. The absence of OB-OA and Amine-OA in the summer data may be due to lower emissions and/or photochemical conversion of these components to OOA.

  7. Laboratory investigation of photochemical oxidation of organic aerosol from wood fires 2: analysis of aerosol mass spectrometer data

    Directory of Open Access Journals (Sweden)

    A. P. Grieshop

    2009-03-01

    Full Text Available Experiments were conducted to investigate the effects of photo-oxidation on organic aerosol (OA in dilute wood smoke by exposing emissions from soft- and hard-wood fires to UV light in a smog chamber. This paper focuses on changes in OA composition measured using a unit-mass-resolution quadrupole Aerosol Mass Spectrometer (AMS. The results highlight how photochemical processing can lead to considerable evolution of the mass, volatility and level of oxygenation of biomass-burning OA. Photochemical oxidation produced substantial new OA, more than doubling the OA mass after a few hours of aging under typical summertime conditions. Aging also decreased the volatility of the OA and made it progressively more oxygenated. The results also illustrate strengths of, and challenges with, using AMS data for source apportionment analysis. For example, the mass spectra of fresh and aged BBOA are distinct from fresh motor-vehicle emissions. The mass spectra of the secondary OA produced from aging wood smoke are very similar to those of the oxygenated OA (OOA that dominates ambient AMS datasets, further reinforcing the connection between OOA and OA formed from photo-chemistry. In addition, aged wood smoke spectra are similar to those from OA created by photo-oxidizing dilute diesel exhaust. This demonstrates that the OOA observed in the atmosphere can be produced by photochemical aging of dilute emissions from different types of combustion systems operating on fuels with modern or fossil carbon. Since OOA is frequently the dominant component of ambient OA, the similarity of spectra of aged emissions from different sources represents an important challenge for AMS-based source apportionment studies.

  8. Chemical profiling and quantification of Gua-Lou-Gui-Zhi decoction by high performance liquid chromatography/quadrupole-time-of-flight mass spectrometry and ultra-performance liquid chromatography/triple quadrupole mass spectrometry.

    Science.gov (United States)

    Xu, Wen; Huang, Mingqing; Li, Huang; Chen, Xianwen; Zhang, Yuqin; Liu, Jie; Xu, Wei; Chu, Kedan; Chen, Lidian

    2015-04-01

    Gua-Lou-Gui-Zhi decoction (GLGZD) is a classical formula of traditional Chinese medicine, which has been commonly used to treat dysfunction after stroke, epilepsy and spinal cord injury. In this study, a systematic method was established for chemical profiling and quantification analysis of the major constituents in GLGZD. For qualitative analysis, a method of high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (Q-TOF MS) was developed. 106 compounds, including monoterpene glycosides, galloyl glucoses, phenolic acids, flavonoids, gingerols and triterpene saponins were identified or tentatively presumed by comparison with reference standards or literature data. According to the qualitative results, a new quantitative analysis method of ultra-performance liquid chromatography/triple quadrupole mass spectrometry (QqQ-MS) was established. 24 representative compounds were simultaneously detected in 10 batches of GLGZD samples in 7.5 min. The calibration curves for all analytes showed good linearity (r>0.9959) within the test ranges. The LODs and the LOQs were less than 30.6 and 70.9 ng/mL, respectively. The RSDs of intra- and inter-day precision, repeatability and stability were below 3.64%, 4.85%, 4.84% and 3.87%, respectively. The overall recoveries ranged from 94.94% to 103.66%, with the RSDs within 5.12%. This study established a high sensitive and efficient method for the integrating quality control, including identification and quantification of Chinese medicinal preparation.

  9. Comparison of a 250 kV single-stage accelerator mass spectrometer with a 5 MV tandem accelerator mass spectrometer--fitness for purpose in bioanalysis.

    Science.gov (United States)

    Young, G C; Corless, S; Felgate, C C; Colthup, P V

    2008-12-01

    The introduction of 'compact' accelerator mass spectrometers into biomedical science, including use in drug metabolism and bioanalytical applications, is an exciting recent development. Comparisons are presented here between a more established and relatively large tandem accelerator which operates at up to 5 MV and a conventional laboratory-sized 250 kV single-stage accelerator mass spectrometer. Biological samples were enriched with low levels of radiocarbon, then converted into graphite prior to analysis on each of the two instruments. The data obtained showed the single-stage instrument to be capable of delivering comparable results, and thus able to provide similar study support, with that provided by the 5 MV instrument, without the significant overheads and complexities which are inherent to the operation of the larger instrument. We believe that the advent of these laboratory-sized accelerator mass spectrometry (AMS) instruments represents a real turning point in the potential for application of AMS by a wider user group.

  10. Highly sensitive and selective analysis of widely targeted metabolomics using gas chromatography/triple-quadrupole mass spectrometry.

    Science.gov (United States)

    Tsugawa, Hiroshi; Tsujimoto, Yuki; Sugitate, Kuniyo; Sakui, Norihiro; Nishiumi, Shin; Bamba, Takeshi; Fukusaki, Eiichiro

    2014-01-01

    In metabolomics studies, gas chromatography coupled with time-of-flight or quadrupole mass spectrometry has frequently been used for the non-targeted analysis of hydrophilic metabolites. However, because the analytical platform employs the deconvolution method to extract single-metabolite information from co-eluted peaks and background noise, the extracted peak is artificial product depending on the mathematical parameters and is not completely compatible with the pure component obtained by analyzing a standard compound. Moreover, it has insufficient ability for quantitative metabolomics. Therefore, highly sensitive and selective methods capable of pure peak extraction without any complicated mathematical techniques are needed. For this purpose, we have developed a novel analytical method using gas chromatography coupled with triple-quadrupole mass spectrometry (GC-QqQ/MS). We developed a selected reaction monitoring (SRM) method to analyze the trimethylsilyl derivatives of 110 metabolites, using electron ionization. This methodology enables us to utilize two complementary techniques-non-targeted and widely targeted metabolomics in the same sample preparation protocol, which would facilitate the formulation or verification of novel hypotheses in biological sciences. The GC-QqQ/MS analysis can accurately identify a metabolite using multichannel SRM transitions and intensity ratios in the analysis of living organisms. In addition, our methodology offers a wide dynamic range, high sensitivity, and highly reproducible metabolite profiles, which will contribute to the biomarker discoveries and quality evaluations in biology, medicine, and food sciences.

  11. Determination of vanillin, ethyl vanillin, and coumarin in infant formula by liquid chromatography-quadrupole linear ion trap mass spectrometry.

    Science.gov (United States)

    Shen, Yan; Han, Chao; Liu, Bin; Lin, Zhengfeng; Zhou, Xiujin; Wang, Chengjun; Zhu, Zhenou

    2014-02-01

    A simple, precise, accurate, and validated liquid chromatography-quadrupole linear ion trap mass spectrometry method was developed for the determination of vanillin, ethyl vanillin, and coumarin in infant formula samples. Following ultrasonic extraction with methanol/water (1:1, vol/vol), and clean-up on an HLB solid-phase extraction cartridge (Waters Corp., Milford, MA), samples were separated on a Waters XSelect HSS T3 column (150 × 2.1-mm i.d., 5-μm film thickness; Waters Corp.), with 0.1% formic acid solution-acetonitrile as mobile phase at a flow rate of 0.25 mL/min. Quantification of the target was performed by the internal standard approach, using isotopically labeled compounds for each chemical group, to correct matrix effects. Data acquisition was carried out in multiple reaction monitoring transitions mode, monitoring 2 multiple reaction monitoring transitions to ensure an accurate identification of target compounds in the samples. Additional identification and confirmation of target compounds were performed using the enhanced product ion modus of the linear ion trap. The novel liquid chromatography-quadrupole linear ion trap mass spectrometry platform offers the best sensitivity and specificity for characterization and quantitative determination of vanillin, ethyl vanillin, and coumarin in infant formula and fulfills the quality criteria for routine laboratory application.

  12. A mass spectrometer with a membrane interface for oil concentration monitoring in seawater

    Science.gov (United States)

    Gorbatskii, V. V.; Elokhin, V. A.; Nikolaev, V. I.; Ershov, T. D.; Elizarov, A. Yu.

    2016-08-01

    An immersion mass spectrometer with a membrane interface was used for oil detection and oil concentration measurements in seawater by measuring in situ the concentrations of three hydrocarbons: benzene, toluene, and xylene in the region of the specialized Primorsk oil loading seaport in the Gulf of Finland. The recorded mass spectra demonstrated the possibility of measuring the oil concentration in seawater and determining the grade of oil products. The use of a mass spectrometer with a membrane separator interface allows measurements of hydrocarbon concentration with high accuracy, which is currently not provided in commercially available monitors.

  13. Validation of a qualitative screening method for pesticides in fruits and vegetables by gas chromatography quadrupole-time of flight mass spectrometry with atmospheric pressure chemical ionization.

    Science.gov (United States)

    Portolés, T; Mol, J G J; Sancho, J V; López, Francisco J; Hernández, F

    2014-08-01

    A wide-scope screening method was developed for the detection of pesticides in fruit and vegetables. The method was based on gas chromatography coupled to a hybrid quadrupole time-of-flight mass spectrometer with an atmospheric pressure chemical ionization source (GC-(APCI)QTOF MS). A non-target acquisition was performed through two alternating scan events: one at low collision energy and another at a higher collision energy ramp (MS(E)). In this way, both protonated molecule and/or molecular ion together with fragment ions were obtained in a single run. Validation was performed according to SANCO/12571/2013 by analysing 20 samples (10 different commodities in duplicate), fortified with a test set of 132 pesticides at 0.01, 0.05 and 0.20mg kg(-1). For screening, the detection was based on one diagnostic ion (in most cases the protonated molecule). Overall, at the 0.01mg kg(-1) level, 89% of the 2620 fortifications made were detected. The screening detection limit for individual pesticides was 0.01mg kg(-1) for 77% of the pesticides investigated. The possibilities for identification according to the SANCO criteria, requiring two ions with a mass accuracy ≤±5ppm and an ion-ratio deviation ≤±30%, were investigated. At the 0.01mg kg(-1) level, identification was possible for 70% of the pesticides detected during screening. This increased to 87% and 93% at the 0.05 and 0.20mg kg(-1) level, respectively. Insufficient sensitivity for the second ion was the main reason for the inability to identify detected pesticides, followed by deviations in mass accuracy and ion ratios.

  14. Toxicological determination and in vitro metabolism of the designer drug methylenedioxypyrovalerone (MDPV) by gas chromatography/mass spectrometry and liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Strano-Rossi, Sabina; Cadwallader, Amy B; de la Torre, Xavier; Botrè, Francesco

    2010-09-01

    A method for the toxicological screening of the new designer drug methylenedioxypyrovalerone (MDPV) is described; with an emphasis on its application for anti-doping analysis. The metabolism of MDPV was evaluated in vitro using human liver microsomes and S9 cellular fractions for CYP450 phase I and uridine 5'-diphosphoglucuronosyltransferase (UGT) and sulfotransferase (SULT) phase II metabolism studies. The resulting metabolites were subsequently liquid/liquid extracted and analyzed using gas chromatography/mass spectrometry (GC/MS) as trimethylsilyl (TMS) derivatives. The structures of the metabolites were further confirmed by accurate mass measurement using a liquid chromatography/quadrupole time-of-flight (LC/QTOF) mass spectrometer. The studies demonstrated that the main metabolites of MDPV are catechol and methyl catechol pyrovalerone, which are in turn sulfated and glucuronated. The method for the determination of MDPV in urine has been fully validated by assessing the limits of detection and quantification, linearity, repeatability, and accuracy. This validation demonstrates the suitability for screening of this stimulant substance for anti-doping and forensic toxicology purposes. 2010 John Wiley & Sons, Ltd.

  15. (r) Mass Resolution versus Chamber Resolution in ALICE Dimuon Forward Spectrometer

    Institute of Scientific and Technical Information of China (English)

    WU Tao

    2007-01-01

    The precisions and its sources of spatial resolutions of tracking chambers and mass resolutions of dimuon signals in ALICE Dimuon Forward Spectrometer are explored by tracking and reconstruction of AliRoot software. The dependences of (r) mass resolution on spatial resolution of tracking chambers are presented with and without background events through simulations.

  16. On the transmission function of an ion-energy and mass spectrometer

    NARCIS (Netherlands)

    Hamers, E. A. G.; van Sark, Wgjhm; Bezemer, J.; W. J. Goedheer,; W.F. van der Weg,

    1998-01-01

    The operation of a mass spectrometer system with an electrostatic energy analyser, designed for measurements of mass-resolved ion-energy distributions, is discussed. We show how the electric fields in the different electrostatic lenses present in the system can be optimized. These lenses direct the

  17. Qualitative analysis of seized synthetic cannabinoids and synthetic cathinones by gas chromatography triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Gwak, Seongshin; Arroyo-Mora, Luis E; Almirall, José R

    2015-02-01

    Designer drugs are analogues or derivatives of illicit drugs with a modification of their chemical structure in order to circumvent current legislation for controlled substances. Designer drugs of abuse have increased dramatically in popularity all over the world for the past couple of years. Currently, the qualitative seized-drug analysis is mainly performed by gas chromatography-electron ionization-mass spectrometry (GC-EI-MS) in which most of these emerging designer drug derivatives are extensively fragmented not presenting a molecular ion in their mass spectra. The absence of molecular ion and/or similar fragmentation pattern among these derivatives may cause the equivocal identification of unknown seized-substances. In this study, the qualitative identification of 34 designer drugs, mainly synthetic cannabinoids and synthetic cathinones, were performed by gas chromatography-triple quadrupole-tandem mass spectrometry with two different ionization techniques, including electron ionization (EI) and chemical ionization (CI) only focusing on qualitative seized-drug analysis, not from the toxicological point of view. The implementation of CI source facilitates the determination of molecular mass and the identification of seized designer drugs. Developed multiple reaction monitoring (MRM) mode may increase sensitivity and selectivity in the analysis of seized designer drugs. In addition, CI mass spectra and MRM mass spectra of these designer drug derivatives can be used as a potential supplemental database along with EI mass spectral database. Copyright © 2014 John Wiley & Sons, Ltd.

  18. Identification of phosphorylation sites of proteins by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The phosphorylation sites of two phosphorylated proteins, bovine b-casein and myelin basic protein (MBP), were identified by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spectrometry (HPLC-ESI-QITMS). The tryptic digest of each protein was separated by HPLC, the molecular weight of each peptide was determined by ESI-QITMS on line, and MS/MS spectrum of each peptide was simultaneously obtained by the combination of collision-induced desorption (CID) technique and tandem mass spectrometry (MS/MS) of QITMS. The phosphorylated peptide was identified by looking into whether the difference between the observed and predicted molecular weights of a peptide is 80 u or its integral multiple. Then the phosphorylation site was identified through manual interpretation of the MS/MS spectrum of the phosphorylated peptide or automatic SEQUEST data base-searching.

  19. Identification of phosphorylation sites of proteins by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    车发云; 邵晓霞; 夏其昌

    2000-01-01

    The phosphorylation sites of two phosphorylated proteins, bovine β-casein and myelin basic protein (MBP), were identified by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spectrometry (HPLC-ESI-QITMS). The tryptic digest of each protein was separated by HPLC, the molecular weight of each peptide was determined by ESI-QITMS on line, and MS/MS spectrum of each peptide was simultaneously obtained by the combination of collision-induced desorption (CID) technique and tandem mass spectrometry (MS/MS) of QITMS. The phosphorylated peptide was identified by looking into whether the difference between the observed and predicted molecular weights of a peptide is 80 u or its integral multiple. Then the phosphorylation site was identified through manual interpretation of the MS/MS spectrum of the phosphorylated peptide or automatic SEQUEST data base-searching.

  20. Performance of the High Resolution, Multi-collector Helix MC Plus Noble Gas Mass Spectrometer at the Australian National University

    Science.gov (United States)

    Zhang, Xiaodong; Honda, Masahiko; Hamilton, Doug

    2016-12-01

    Performance of the Helix MC Plus noble gas mass spectrometer installed at the Australian National University (ANU) is reported. Results for sensitivity, mass discrimination and their linearity against partial pressure of noble gases, and mass resolution of the mass spectrometer are presented, and the results are compared with those of conventional noble gas mass spectrometers. The application of the five detectors on the Helix MC Plus in measuring various noble gas isotopes in multi-collector modes and the integration of the software drivers of peripheral hardware devices into the controlling program Qtegra of the mass spectrometer are discussed. High mass resolution (>1800) and mass resolving power (>8000) make this mass spectrometer unique in noble gas cosmo-geochemistry. It provides the capability to measure isobaric interference-free noble gas isotopes in multi-collector mode, significantly improves the accuracy to determine isotopic ratios, and greatly increases the efficiency of data acquisition.

  1. Performance of the High Resolution, Multi-collector Helix MC Plus Noble Gas Mass Spectrometer at the Australian National University

    Science.gov (United States)

    Zhang, Xiaodong; Honda, Masahiko; Hamilton, Doug

    2016-09-01

    Performance of the Helix MC Plus noble gas mass spectrometer installed at the Australian National University (ANU) is reported. Results for sensitivity, mass discrimination and their linearity against partial pressure of noble gases, and mass resolution of the mass spectrometer are presented, and the results are compared with those of conventional noble gas mass spectrometers. The application of the five detectors on the Helix MC Plus in measuring various noble gas isotopes in multi-collector modes and the integration of the software drivers of peripheral hardware devices into the controlling program Qtegra of the mass spectrometer are discussed. High mass resolution (>1800) and mass resolving power (>8000) make this mass spectrometer unique in noble gas cosmo-geochemistry. It provides the capability to measure isobaric interference-free noble gas isotopes in multi-collector mode, significantly improves the accuracy to determine isotopic ratios, and greatly increases the efficiency of data acquisition.

  2. Laboratory investigation of photochemical oxidation of organic aerosol from wood fires – Part 2: Analysis of aerosol mass spectrometer data

    Directory of Open Access Journals (Sweden)

    A. P. Grieshop

    2008-09-01

    Full Text Available Experiments were conducted to investigate the effects of photo-oxidation on organic aerosol (OA in dilute wood smoke by exposing emissions from soft- and hard-wood fires to UV light in a smog chamber. This paper focuses on changes in OA composition measured using a unit mass resolution quadrupole Aerosol Mass Spectrometer (AMS. The results highlight how photochemical processing can lead to considerable evolution of the mass, the volatility and the level of oxygenation of biomass-burning OA. Photochemical oxidation produced substantial new OA, more than doubling the primary contribution after a few hours of aging under typical summertime conditions. Aging decreased the OA volatility of the total OA as measured with a thermodenuder; it also made the OA progressively more oxygenated in every experiment. With explicit knowledge of the condensed-phase mass spectrum (MS of the primary emissions from each fire, each MS can be decomposed into primary and residual spectra throughout the experiment. The residual spectra provide an estimate of the composition of the photochemically produced OA. These spectra are also very similar to those of the oxygenated OA that dominates ambient AMS datasets. In addition, aged wood smoke spectra are shown to be similar to those from OA created by photo-oxidized dilute diesel exhaust and aged biomass-burning OA measured in urban and remote locations. This demonstrates that the oxygenated OA observed in the atmosphere can be produced by photochemical aging of dilute emissions from combustion of fuels containing both modern and fossil carbon.

  3. Tandem Mass Spectrometry on a Miniaturized Laser Desorption Time-of-Flight Mass Spectrometer

    Science.gov (United States)

    Li, Xiang; Cornish, Timothy; Getty, Stephanie A.; Brinckerhoff, William B.

    2016-01-01

    Tandem mass spectrometry (MSMS) is a powerful and widely-used technique for identifying the molecular structure of organic constituents of a complex sample. Application of MSMS to the study of unknown planetary samples on a remote space mission would contribute to our understanding of the origin, evolution, and distribution of extraterrestrial organics in our solar system. Here we report on the realization of MSMS on a miniaturized laser desorption time-of-flight mass spectrometer (LD-TOF-MS), which is one of the most promising instrument types for future planetary missions. This achievement relies on two critical components: a curved-field reflectron and a pulsed-pin ion gate. These enable use of the complementary post-source decay (PSD) and laser-assisted collision induced dissociation (L-CID) MSMS methods on diverse measurement targets with only modest investment in instrument resources such as volume and weight. MSMS spectra of selected molecular targets in various organic standards exhibit excellent agreement when compared with results from a commercial, laboratory-scale TOF instrument, demonstrating the potential of this powerful technique in space and planetary environments.

  4. A cheap and compact mass spectrometer for radioactive ions based on a Wien filter

    Science.gov (United States)

    Pierret, C.; Maunoury, L.; Pacquet, J. Y.; Saint-Laurent, M.-G.; Tuske, O.

    2008-10-01

    This paper presents simulations of a mass spectrometer composed of one or two Wien filters. The ion source used is MONO1000 ECRIS. This ion source can produce singly charged ions with high efficiency, especially for gaseous materials. After extraction, the ions are mass selected and can be injected either into a beam line towards an experiment area or in an N+ charge booster. Due to its compactness and simplicity the proposed spectrometer is well adapted for preparing and analyzing radioactive beams. The simulations are based on the SIMION 3D [www.simion.com/] software.

  5. A cheap and compact mass spectrometer for radioactive ions based on a Wien filter

    Energy Technology Data Exchange (ETDEWEB)

    Pierret, C. [CIRIL, CEA/DSM CNRS/IN2P3, Avenue Henri Becquerel, B.P. 5133, F-14070 Caen cedex 05 (France)], E-mail: Pierret@ganil.fr; Maunoury, L. [CIRIL, CEA/DSM CNRS/IN2P3, Avenue Henri Becquerel, B.P. 5133, F-14070 Caen cedex 05 (France); Pacquet, J.Y.; Saint-Laurent, M.-G. [GANIL, CEA/DSM CNRS/IN2P3, Boulevard Henri Becquerel, B.P. 55027, F-14076 Caen cedex 05 (France); Tuske, O. [CEA/Saclay, DSM/DAPNIA, 91191 Gif/Yvette (France)

    2008-10-15

    This paper presents simulations of a mass spectrometer composed of one or two Wien filters. The ion source used is MONO1000 ECRIS. This ion source can produce singly charged ions with high efficiency, especially for gaseous materials. After extraction, the ions are mass selected and can be injected either into a beam line towards an experiment area or in an N{sup +} charge booster. Due to its compactness and simplicity the proposed spectrometer is well adapted for preparing and analyzing radioactive beams. The simulations are based on the SIMION 3D [ (http://www.simion.com/)] software.

  6. Simultaneous qualitative and quantitative analysis of 21 mycotoxins in Radix Paeoniae Alba by ultra-high performance liquid chromatography quadrupole linear ion trap mass spectrometry and QuEChERS for sample preparation.

    Science.gov (United States)

    Xing, Yanyan; Meng, Wenting; Sun, Wanyang; Li, Dongxiang; Yu, Zhiguo; Tong, Ling; Zhao, Yunli

    2016-09-15

    A high-throughput method for simultaneous qualitative and quantitative analysis of 21 mycotoxins in Radix Paeoniae Alba (RPA) was developed by coupling the modified QuEChERS method with ultra-high performance liquid chromatography quadrupole linear ion trap mass spectrometry (UHPLC-QqLIT-MS). The 21 mycotoxins were extracted and cleaned up using QuEChERS-based procedure, then further separated on a C18 column and detected by a hybrid triple quadrupole linear ion trap mass spectrometer equipped with electrospray ionization source in the multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode. Under this technique, 13 mycotoxins were detected using acetonitrile and water containing 0.1% formic acid as the mobile phase in positive mode while the other 8 mycotoxins were detected using acetonitrile and water containing 0.1% ammonia as the mobile phase in negative mode. The calibration curves of all analytes showed good linearity (r(2)>0.995) within test ranges. The limits of detection and quantification ranged from 0.031 to 5.4μg/kg and 0.20 to 22μg/kg, respectively. Additionally, recoveries were all above 75.3% with relative standard deviations within 15%. The method proposed herein with significant advantages including simple pretreatment, rapid determination as well as high sensitivity, accuracy and throughput would be a preferred candidate for the determination and quantification of multi-class mycotoxin contaminants in real samples.

  7. Qualitative and Quantitative Analysis of Major Triterpenoids in Alismatis Rhizoma by High Performance Liquid Chromatography/Diode-Array Detector/Quadrupole-Time-of-Flight Mass Spectrometry and Ultra-Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Wanli Zhao

    2015-07-01

    Full Text Available Alismatis Rhizoma (AMR is a well-known natural medicine with a long history in Chinese medicine and has been commonly used for treating a wide range of ailments related to dysuria, edema, nephropathy, hyperlipidaemia, diabetes, inflammation as well as tumors in clinical applications. Most beneficial effects of AMR are attributed to the presence of protostane terpenoids, the major active ingredients of Alismatis Rhizoma (AMR. In this study, a systematic high performance liquid chromatography/diode-array detector/quadrupole-time-of-flight mass spectrometry (HPLC-DAD-Q-TOF MS and ultra-performance liquid chromatography/triple quadrupole mass spectrometry (UPLC-QqQ MS method was developed for qualitative and quantitative analyses of the major AMR triterpenoids. First, a total of 25 triterpenoid components, including 24 known compounds and one new compound were identified by comparison with UV spectra, molecular ions and fragmentation behaviors of reference standards or the literature. Second, an efficient method was established for the rapid simultaneous determination of 14 representative triterpenoids by UPLC-QqQ MS. Forty-three batches of AMR were analyzed with linearity (r, 0.9980–0.9999, intra-day precision (RSD, 1.18%–3.79%, inter-day precision (RSD, 1.53%–3.96%, stability (RSD, 1.32%–3.97%, repeatability (RSD, 2.21%–4.25%, and recovery (98.11%–103.8%. These results indicated that new approaches combining HPLC-DAD-Q-TOF MS and UPLC-QqQ MS are applicable in the qualitative and quantitative analysis of AMR.

  8. Cross contamination in dual inlet isotope ratio mass spectrometers

    NARCIS (Netherlands)

    Meijer, H.A.J.; Neubert, R.E.M.; Visser, G.H.

    2000-01-01

    Since the early days of geochemical isotope ratio mass spectrometry there has always been the problem of cross contamination, i.e. the contamination of the sample gas with traces of reference gas land vice versa) in a dual inlet system and the analyzer itself. This was attributable to valve leakages

  9. Method for selective detection of explosives in mass spectrometer or ion mobility spectrometer at parts-per-quadrillion level

    Science.gov (United States)

    Ewing, Robert G.; Atkinson, David A.; Clowers, Brian H.

    2015-09-01

    A method for selective detection of volatile and non-volatile explosives in a mass spectrometer or ion mobility spectrometer at a parts-per-quadrillion level without preconcentration is disclosed. The method comprises the steps of ionizing a carrier gas with an ionization source to form reactant ions or reactant adduct ions comprising nitrate ions (NO.sub.3.sup.-); selectively reacting the reactant ions or reactant adduct ions with at least one volatile or non-volatile explosive analyte at a carrier gas pressure of at least about 100 Ton in a reaction region disposed between the ionization source and an ion detector, the reaction region having a length which provides a residence time (tr) for reactant ions therein of at least about 0.10 seconds, wherein the selective reaction yields product ions comprising reactant ions or reactant adduct ions that are selectively bound to the at least one explosive analyte when present therein; and detecting product ions with the ion detector to determine presence or absence of the at least one explosive analyte.

  10. Probe Heating Method for the Analysis of Solid Samples Using a Portable Mass Spectrometer.

    Science.gov (United States)

    Kumano, Shun; Sugiyama, Masuyuki; Yamada, Masuyoshi; Nishimura, Kazushige; Hasegawa, Hideki; Morokuma, Hidetoshi; Inoue, Hiroyuki; Hashimoto, Yuichiro

    2015-01-01

    We previously reported on the development of a portable mass spectrometer for the onsite screening of illicit drugs, but our previous sampling system could only be used for liquid samples. In this study, we report on an attempt to develop a probe heating method that also permits solid samples to be analyzed using a portable mass spectrometer. An aluminum rod is used as the sampling probe. The powdered sample is affixed to the sampling probe or a droplet of sample solution is placed on the tip of the probe and dried. The probe is then placed on a heater to vaporize the sample. The vapor is then introduced into the portable mass spectrometer and analyzed. With the heater temperature set to 130°C, the developed system detected 1 ng of methamphetamine, 1 ng of amphetamine, 3 ng of 3,4-methylenedioxymethamphetamine, 1 ng of 3,4-methylenedioxyamphetamine, and 0.3 ng of cocaine. Even from mixtures consisting of clove powder and methamphetamine powder, methamphetamine ions were detected by tandem mass spectrometry. The developed probe heating method provides a simple method for the analysis of solid samples. A portable mass spectrometer incorporating this method would thus be useful for the onsite screening of illicit drugs.

  11. Mobile mass spectrometer for determination of heavy metals in sea water: Numerical simulation and experimental verification

    Science.gov (United States)

    Kogan, V. T.; Pavlov, A. K.; Chichagov, Yu. V.; Tubol'Tsev, Yu. V.; Savchenko, M. I.; Smirnov, O. B.; Viktorova, O. S.; Viktorov, I. V.; Vlasov, S. A.; Dubenskiĭ, B. M.; Nedvigin, V.; Gao, Ya.

    2007-12-01

    A prototype mobile mass spectrometer for direct detection of heavy metal traces in water is proposed. The instrument allows automated dosed injection of liquid samples (2.5 20.0 μl) into the lock vacuum chamber of the instrument, extraction of salts containing target components for their following introduction into the high-vacuum chamber of the instrument, and determination of the component concentrations in the initial sample by means of a portable magnetic mass spectrometer equipped with an original electron-impact ion source. Experimental testing of the spectrometer using aqueous solutions containing Zn, Fe, Cu, As, and Cd shows that the instrument can detect heavy metals in water, including salt water, at concentrations ranging from 1 mg/l to 10 μg/l. The experimental results are discussed.

  12. Energy-resolved depth profiling of metal-polymer interfaces using dynamic quadrupole secondary ion mass spectrometry.

    Science.gov (United States)

    Téllez, Helena; Vadillo, José M; Laserna, J Javier

    2009-08-01

    Quadrupole secondary ion mass spectrometry (qSIMS) characterization of a metallized polypropylene film used in the manufacturing of capacitors has been performed. Ar(+) primary ions were used to preserve the oxidation state of the surface. The sample exhibits an incomplete metallization that made it difficult to determine the exact location of the metal-polymer interface due to the simultaneous contribution of ions with identical m/z values from the metallic and the polymer layers. Energy filtering by means of a 45 degrees electrostatic analyzer allowed resolution of the metal-polymer interface by selecting a suitable kinetic energy corresponding to the ions generated in the metallized layer but not from the polymer. Under these conditions, selective analyses of isobaric interferences such as (27)Al(+) and (27)C(2)H(3) (+) or (43)AlO(+) and (43)C(3)H(7) (+) have been successfully performed.

  13. Simultaneous determination of 24 constituents in Cortex Lycii using high-performance liquid chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Zhang, Jing-Xian; Guan, Shu-Hong; Yang, Min; Feng, Rui-Hong; Wang, Yang; Zhang, Yi-Bei; Chen, Xin; Chen, Xiao-Hui; Bi, Kai-Shun; Guo, De-An

    2013-04-15

    A fast high-performance liquid chromatography (HPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry method was developed to determine 24 components including 11 phenolic compounds, 9 phenolic amides, and 4 cyclic peptides in Cortex Lycii. The analytes were quantified by a triple quadrupole instrument in multiple reaction monitoring (MRM) mode. The fragmentation patterns of phenolic amides and cyclic peptides using ESI and collision-induced dissociation (CID) techniques are reported. This assay method was validated with respect to linearity (r(2)>0.9920), precision, repeatability, and accuracy (recovery rate between 93.0 and 105.9% with RSDPrinciple component analysis (PCA) was used to discriminate samples from different geographical regions of China, and cyclic peptides were considered to be the chemical markers responsible for the classification. The systematic and integrated assessment of Cortex Lycii provides sufficient evidence for the establishment of the quality standard.

  14. Dithranol as a matrix for matrix assisted laser desorption/ionization imaging on a fourier transform ion cyclotron resonance mass spectrometer.

    Science.gov (United States)

    Le, Cuong H; Han, Jun; Borchers, Christoph H

    2013-11-26

    Mass spectrometry imaging (MSI) determines the spatial localization and distribution patterns of compounds on the surface of a tissue section, mainly using MALDI (matrix assisted laser desorption/ionization)-based analytical techniques. New matrices for small-molecule MSI, which can improve the analysis of low-molecular weight (MW) compounds, are needed. These matrices should provide increased analyte signals while decreasing MALDI background signals. In addition, the use of ultrahigh-resolution instruments, such as Fourier transform ion cyclotron resonance (FTICR) mass spectrometers, has the ability to resolve analyte signals from matrix signals, and this can partially overcome many problems associated with the background originating from the MALDI matrix. The reduction in the intensities of the metastable matrix clusters by FTICR MS can also help to overcome some of the interferences associated with matrix peaks on other instruments. High-resolution instruments such as the FTICR mass spectrometers are advantageous as they can produce distribution patterns of many compounds simultaneously while still providing confidence in chemical identifications. Dithranol (DT; 1,8-dihydroxy-9,10-dihydroanthracen-9-one) has previously been reported as a MALDI matrix for tissue imaging. In this work, a protocol for the use of DT for MALDI imaging of endogenous lipids from the surfaces of mammalian tissue sections, by positive-ion MALDI-MS, on an ultrahigh-resolution hybrid quadrupole FTICR instrument has been provided.

  15. A Method for Estimating Mass-Transfer Coefficients in a Biofilter from Membrane Inlet Mass Spectrometer Data

    DEFF Research Database (Denmark)

    Nielsen, Anders Michael; Nielsen, Lars Peter; Feilberg, Anders;

    2009-01-01

    A membrane inlet mass spectrometer (MIMS) was used in combination with a developed computer model to study and improve management of a biofilter (BF) treating malodorous ventilation air from a meat rendering facility. The MIMS was used to determine percentage removal efficiencies (REs) of selected...

  16. Plutonium ion emission from carburized rhenium mass spectrometer filaments

    Energy Technology Data Exchange (ETDEWEB)

    Kelley, J.M.; Robertson, D.M.

    1985-01-01

    Physicochemical processes important to the application of thermal emission mass spectrometry were identified and clarified. Effects of filament carbon concentration and temperature on plutonium ion emissions from a carburized rhenium filament were determined. Filament carbon concentration profoundly affected the appearance and duration of an ion signal. A useful ion signal was produced only when the carbon saturation temperature of the filament was exceeded, at which point first-order kinetics were either achieved or closely approached. This paper explains observed ion emission behavior in terms of pausible carbothermic reduction reactions and carbon diffusion processes that direct the course of those reactions. 31 references, 5 figures.

  17. High-performance hybrid Orbitrap mass spectrometers for quantitative proteome analysis

    DEFF Research Database (Denmark)

    Williamson, James C; Edwards, Alistair V G; Verano-Braga, Thiago;

    2016-01-01

    We present basic workups and quantitative comparisons for two current generation Orbitrap mass spectrometers, the Q Exactive Plus and Orbitrap Fusion Tribrid, which are widely considered two of the highest performing instruments on the market. We assessed the performance of two quantitative methods...

  18. A Miniature Mass Spectrometer for High-Flux Cosmic Dust Analysis

    Science.gov (United States)

    Austin, D. E.; Manning, H. L. K.; Beauchamp, J. L.

    2007-03-01

    We designed a novel mass spectrometer for in situ characterization of micro-particulates in regions of high concentration, such as a comet fly-by, planetary ring, or impact-generated plume. This device is based on novel ion optics that allow high performa

  19. Improving mass spectrometer sensitivity using a high-pressure electrodynamic ion funnel interface.

    Science.gov (United States)

    Ibrahim, Yehia; Tang, Keqi; Tolmachev, Aleksey V; Shvartsburg, Alexandre A; Smith, Richard D

    2006-09-01

    We report on a new electrodynamic ion funnel that operates at a pressure of 30 torr with no loss of ion transmission. The enhanced performance compared with previous ion funnel designs optimized for pressures of multicapillary inlet, the interface provided more efficient introduction of ions, resulting in a significant enhancement in mass spectrometer sensitivity and detection limits.

  20. MEMS Fabrication of Micro Cylindrical Ion Trap Mass Spectrometer for CubeSats Application

    Science.gov (United States)

    Zheng, Y.

    2015-10-01

    Microelectromechanical Systems (MEMS) technology is used to fabricate arrays of micro Cylindrical Ion Traps (μCIT) which are integrated into a miniaturized mass spectrometer (MS). The micro μCITs are built from silicon wafers and requires high machining precision, smooth surface, and high dimensional uniformity across the array for optimum mass spectrometer performance. In order to build these 3D miniature structures several MEMS processing techniques were explored and a process was developed and tested. By using the developed MEMS process, the required μCIT 4 x 4 arrays were fabricated. This included a chip design variation in which mechanical locking pits and posts were machined in the Ring Electrode (RE) chip and End Plate (EP) chips respectively, for self-assembly. The size of the assembled μCIT is only 12 mm x 12 mm x 1.5 mm. It is a key component for the miniature mass spectrometer. The micro cylindrical ion trap mass spectrometer has the advantages of low-power operation, simpler electronics and less-stringent vacuum system requirements. The MEMS batch production capabilities will also greatly lower the cost. It is a promising candidate for CubeSat and nanoSats applications for exploration of chemical distributions in space.

  1. Development of a high vacuum sample preparation system for helium mass spectrometer

    Science.gov (United States)

    Kumar, P.; Das, N. K.; Mallik, C.; Bhandari, R. K.

    2012-11-01

    A high vacuum sample preparation system for the 3He/4He ratio mass spectrometer (Helix SFT) has been developed to remove all the gaseous constituents excluding helium from the field gases. The sample preparation system comprises of turbo molecular pump, ion pump, zirconium getter, pipettes and vacuum gauges with controller. All these are fitted with cylindrical SS chamber using all metal valves. The field samples are initially treated with activated charcoal trap immersed in liquid nitrogen to cutoff major impurities and moisture present in the sample gas. A sample of 5 ml is collected out of this stage at a pressure of 10-2 mbar. This sample is subsequently purified at a reduced pressure of 10-7 mbar before it is injected into the ion source of the mass spectrometer. The sample pressure was maintained below 10-7 mbar with turbo molecular vacuum pumps and ion pumps. The sample gas passes through several getter elements and a cold finger with the help of manual high vacuum valves before it is fed to the mass spectrometer. Thus the high vacuum sample preparation system introduces completely clean, dry and refined helium sample to the mass spectrometer for best possible analysis of isotopic ratio of helium.

  2. Ultrasensitive resonance ionization mass spectrometer for evaluating krypton contamination in xenon dark matter detectors

    Energy Technology Data Exchange (ETDEWEB)

    Iwata, Y., E-mail: iwata.yoshihiro@jaea.go.jp [Experimental Fast Reactor Department, Oarai Research and Development Center, Japan Atomic Energy Agency, 4002 Narita, Oarai, Ibaraki 311-1393 (Japan); Sekiya, H. [Kamioka Observatory, Institute for Cosmic Ray Research, The University of Tokyo, Higashi-Mozumi, Kamioka, Hida, Gifu 506-1205 (Japan); Kavli Institute for the Physics and Mathematics of the Universe, The University of Tokyo, Kashiwa, Chiba 277-8582 (Japan); Ito, C. [Experimental Fast Reactor Department, Oarai Research and Development Center, Japan Atomic Energy Agency, 4002 Narita, Oarai, Ibaraki 311-1393 (Japan)

    2015-10-11

    An ultrasensitive resonance ionization mass spectrometer that can be applied to evaluate krypton (Kr) contamination in xenon (Xe) dark matter detectors has been developed for measuring Kr at the parts-per-trillion (ppt) or sub-ppt level in Xe. The gas sample is introduced without any condensation into a time-of-flight mass spectrometer through a pulsed supersonic valve. Using a nanosecond pulsed laser at 212.6 nm, {sup 84}Kr atoms in the sample are resonantly ionized along with other Kr isotopes. {sup 84}Kr ions are then mass separated and detected by the mass spectrometer in order to measure the Kr impurity concentration. With our current setup, approximately 0.4 ppt of Kr impurities contained in pure argon (Ar) gas are detectable with a measurement time of 1000 s. Although Kr detection sensitivity in Xe is expected to be approximately half of that in Ar, our spectrometer can evaluate Kr contamination in Xe to the sub-ppt level.

  3. FY16 Safeguards Technology Cart-Portable Mass Spectrometer Project Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Cyril V. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Whitten, William B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-02-01

    The Oak Ridge National Laboratory project for the Next Generation Safeguards Initiative Safeguards Technology Development Subprogram has been involved in the development of a cart portable mass spectrometer based on a Thermo ITQ ion trap mass spectrometer (referred to simply as the ITQ) for the field analysis of 235U/238U ratios in UF6. A recent discovery of the project was that combining CO2 with UF6 and introducing the mixture to the mass spectrometer (MS) appeared to increase the ionization efficiency and, thus, reduce the amount of UF6 needed for an analysis while also reducing the corrosive effects of the sample. However, initial experimentation indicated that mixing parameters should be closely controlled to ensure reproducible results. To this end, a sample manifold (SM) that would ensure the precise mixing of UF6 and CO2 was designed and constructed. A number of experiments were outlined and conducted to determine optimum MS and SM conditions which would provide the most stable isotope ratio analysis. The principal objective of the project was to provide a retrofit ITQ mass spectrometer operating with a SM capable of achieving a variation in precision of less than 1% over 1 hour of sampling. This goal was achieved by project end with a variation in precision of 0.5 to 0.8% over 1 hour of sampling.

  4. High precision electric gate for time-of-flight ion mass spectrometers

    Science.gov (United States)

    Sittler, Edward C. (Inventor)

    2011-01-01

    A time-of-flight mass spectrometer having a chamber with electrodes to generate an electric field in the chamber and electric gating for allowing ions with a predetermined mass and velocity into the electric field. The design uses a row of very thin parallel aligned wires that are pulsed in sequence so the ion can pass through the gap of two parallel plates, which are biased to prevent passage of the ion. This design by itself can provide a high mass resolution capability and a very precise start pulse for an ion mass spectrometer. Furthermore, the ion will only pass through the chamber if it is within a wire diameter of the first wire when it is pulsed and has the right speed so it is near all other wires when they are pulsed.

  5. A novel solid-phase extraction for the concentration of sweeteners in water and analysis by ion-pair liquid chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Gan, Zhiwei; Sun, Hongwen; Wang, Ruonan; Feng, Biting

    2013-01-25

    A highly sensitive method for the simultaneous trace (ng/L) quantification of seven commonly used artificial sweeteners in a variety of water samples using solid-phase extraction and ion-pair high-performance liquid chromatography (HPLC) triple quadrupole mass spectrometer with an electrospray ionization source (ESI-MS) in negative ion multiple reaction monitoring mode was developed. Ten solid phase extraction (SPE) cartridges were tested to evaluate their applicability for the pre-concentration of the analytes, and their loading and eluting parameters were optimized. Satisfactory recoveries (77-99%) of all of the studied sweeteners were obtained using a Poly-Sery PWAX cartridge with 25 mM sodium acetate solution (pH 4) as wash buffer and methanol containing 1mM tris (hydroxymethyl) amino methane (TRIS) as eluent. The method is sound and does not require pH adjustment or buffering of water samples. The HPLC separation was performed on an Athena C18-WP column with water and acetonitrile, both containing 5mM ammonium acetate and 1mM TRIS as mobile phases, in gradient elution mode. The linearity, precision, and accuracy of the method were evaluated, and good reproducibility was obtained. Method quantification limits varied between 0.4 and 7.5 ng/L for different water samples. The post-extraction spike method was applied to assess matrix effects, and quantification was achieved using internal standard calibration to overcome the unavoidable matrix effects during ESI-MS analysis. The method was applied to the analysis of thirteen water samples from Tianjin, China, including wastewater, tap water, surface water, and groundwater. The method described here is time-saving, accurate and precise, and is suitable for monitoring artificial sweeteners in different water matrices.

  6. Evaluation of lead isotope compositions of NIST NBS 981 measured by thermal ionization mass spectrometer and multiple-collector inductively coupled plasma mass spectrometer

    Directory of Open Access Journals (Sweden)

    Honglin Yuan

    2016-09-01

    Full Text Available Because Pb isotopes can be used for tracing, they are widely used in many disciplines. The detection and analysis of Pb isotopes of bulk samples are usually conducted using thermal ionization mass spectrometer (TIMS and multiple-collector inductively coupled plasma mass spectrometer (MC-ICP-MS, both of which need external reference materials with known isotopic compositions to correct for the mass discrimination effect produced during analysis. NIST NBS 981 is the most widely used reference material for Pb isotope analysis; however, the isotopic compositions reported by various analytical laboratories, especially those using TIMS, vary from each other. In this study, we statistically evaluated 229 reported TIMS analysis values collected by GeoReM in the last 30 years, 176 reported MC-ICP-MS analysis values, and 938 MC-ICP-MS analysis results from our laboratory in the last five years. After careful investigation, only 40 TIMS results were found to have double or triple spikes. The ratios of the overall weighted averages, 206Pb/204Pb, 207Pb/204Pb, and 208Pb/204Pb, obtained from 40 spiked TIMS reports and 1114 MC-ICP-MS results of NIST NBS 981 isotopes were 16.9406 ± 0.0003 (2s, 15.4957 ± 0.0002 (2s, and 36.7184 ± 0.0007 (2s, respectively.

  7. Analysis of ion dynamics and peak shapes for delayed extraction time-of-flight mass spectrometers

    Science.gov (United States)

    Collado, V. M.; Ponciano, C. R.; Fernandez-Lima, F. A.; da Silveira, E. F.

    2004-06-01

    The dependence of time-of-flight (TOF) peak shapes on time-dependent extraction electric fields is studied theoretically. Conditions for time focusing are analyzed both analytically and numerically for double-acceleration-region TOF spectrometers. Expressions for the spectrometer mass resolution and for the critical delay time are deduced. Effects due to a leakage field in the first acceleration region are shown to be relevant under certain conditions. TOF peak shape simulations for the delayed extraction method are performed for emitted ions presenting a Maxwellian initial energy distribution. Calculations are compared to experimental results of Cs+ emission due to CsI laser ablation.

  8. Influence of the Ion Source Operating Conditions on the Characteristics of a Prism Mass Spectrometer With Inhomogeneous Magnetic Field

    Directory of Open Access Journals (Sweden)

    P.O. Kuzema

    2010-01-01

    Full Text Available The influence of magnetic field focusing the electron beam in ion source of mass spectrometer on the analytical characteristics of the instrument has been studied. The range of current of ion source's focusing electromagnet providing the optimal performance of the mass spectrometer has been determined.

  9. Development of Localized Plasma Etching System for Failure Analyses in Semiconductor Devices: (3)Etching-Monitoring Using Quadrupole Mass Spectrometry

    Science.gov (United States)

    Takahashi, Satoshi; Horie, Tomoyuki; Shirayama, Yuya; Yokosuka, Shuntaro; Kashimura, Kenta; Hayashi, Akihiro; Iwase, Chikatsu; Shimbori, Shun'ichiro; Tokumoto, Hiroshi; Naitoh, Yasuhisa; Shimizu, Tetsuo

    Quadrupole mass spectrometry (QMS) has been applied to monitor the etching processes in a localized plasma etching system. An inward plasma was employed for etching in which the etching gas was discharged in the narrow gap between the etched sample and the entrance of an evacuating capillary tube. As the etching products are immediately evacuated through the capillary, a QMS system equipped at the capillary exit is able to analyze the products without any loss in concentration via diffusion into the chamber. Two kinds of samples, thermally grown SiO2 on Si and spin-coated polyimide film on Si, were etched, and the chemical species in the evacuated etching gas were analyzed with QMS, which enables monitoring of the composition of the surface being etched. Samples of thermal SiO2 were etched with CF4 plasma. The peak height of the SiF3+ signal during the SiO2 etching was lower than that observed during etching of the silicon substrate, leading to endpoint detection. The endpoint detection of the polyimide film etching was conducted using two etching gases: pure O2 and pure CF4. When O2 was used, the endpoint was detected by the decrease of the mass peak attributed to CO. When CF4 was employed, the plasma was able to etch both the polyimide film and Si substrate. Then the endpoint was detected by the increase of the mass peak of SiF3+ produced by the etching of the Si substrate.

  10. New Potential Biomarker for Methasterone Misuse in Human Urine by Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry

    Science.gov (United States)

    Zhang, Jianli; Lu, Jianghai; Wu, Yun; Wang, Xiaobing; Xu, Youxuan; Zhang, Yinong; Wang, Yan

    2016-01-01

    In this study, methasterone urinary metabolic profiles were investigated by liquid chromatography quadrupole time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. A healthy male volunteer was asked to take the drug and liquid–liquid extraction was employed to process urine samples. Chromatographic peaks for potential metabolites were hunted out with the theoretical [M − H]− as a target ion in a full scan experiment and actual deprotonated ions were studied in targeted MS/MS experiment. Fifteen metabolites including two new sulfates (S1 and S2), three glucuronide conjugates (G2, G6 and G7), and three free metabolites (M2, M4 and M6) were detected for methasterone. Three metabolites involving G4, G5 and M5 were obtained for the first time in human urine samples. Owing to the absence of helpful fragments to elucidate the steroid ring structure of methasterone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was employed to obtain structural information of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and the potential structure was inferred using a combined MS method. Metabolite detection times were also analyzed and G2 (18-nor-17β-hydroxymethyl-2α, 17α-dimethyl-androst-13-en-3α-ol-ξ-O-glucuronide) was thought to be new potential biomarker for methasterone misuse which can be detected up to 10 days. PMID:27669235

  11. Iodine-xenon studies and the relax mass spectrometer

    Science.gov (United States)

    Gilmour, J. D.; Ash, R. D.; Lyon, I. C.; Johnston, W. A.; Hutchison, R.; Bridges, J. C.; Turner, G.

    1994-07-01

    RELAX combines a resonance ionization ion source with a cryogenic sample concentrator to achieve ultrasensitivity. Gas is extracted from samples using either a continuous wave laser microprobe based on an argon-ion laser or a filament microfurnace. Recent refinements in the operating procedure have resulted in optimum sensitivities such that detection rates of 1 cps are achieved from fewer than 500 atoms. A Xe-128 spike reservoir has also been added and characterized, allowing accurate determinations of absolute amounts of gas. We have completed a preliminary study of the iodine-xenon system in samples from the Bjurbole and Parnallee meteorites. Bjurbole chondrules ranging in mass from 5.45 mg to 260 micrograms were analyzed by laser microprobe. The results from these samples are consistent with an effectively uniform formation age, suggesting that the use of Bjurbole chondrules for calibration of this chronometer can be extended to samples in this size range. Samples from two chondrules from the Parnallee meteorite have been analyzed to date. An alpha-cristobalite-bearing chondrule (designated CB1) was found to have a formation age 4.62 +/- 0.44 Ma after Bjurboele, while a porphyritic olivine macrochondrule appears to have been reset after the decay of I-129(t1/2 17 Ma). Consideration of these results alongside Ar-Ar data from the macrochondrule and whole rock samples suggests that Parnallee has a complex history: The macrochondrule underwent an early postcrystallization degassing event but appears to have been essentially unaffected by the later (1.9 Ga) partial resetting of the bulk meteorite.

  12. TEMPO-Assisted Free Radical-Initiated Peptide Sequencing Mass Spectrometry (FRIPS MS) in Q-TOF and Orbitrap Mass Spectrometers: Single-Step Peptide Backbone Dissociations in Positive Ion Mode

    Science.gov (United States)

    Jang, Inae; Lee, Sun Young; Hwangbo, Song; Kang, Dukjin; Lee, Hookeun; Kim, Hugh I.; Moon, Bongjin; Oh, Han Bin

    2017-01-01

    The present study demonstrates that one-step peptide backbone fragmentations can be achieved using the TEMPO [2-(2,2,6,6-tetramethyl piperidine-1-oxyl)]-assisted free radical-initiated peptide sequencing (FRIPS) mass spectrometry in a hybrid quadrupole time-of-flight (Q-TOF) mass spectrometer and a Q-Exactive Orbitrap instrument in positive ion mode, in contrast to two-step peptide fragmentation in an ion-trap mass spectrometer (reference Anal. Chem. 85, 7044-7051 (30)). In the hybrid Q-TOF and Q-Exactive instruments, higher collisional energies can be applied to the target peptides, compared with the low collisional energies applied by the ion-trap instrument. The higher energy deposition and the additional multiple collisions in the collision cell in both instruments appear to result in one-step peptide backbone dissociations in positive ion mode. This new finding clearly demonstrates that the TEMPO-assisted FRIPS approach is a very useful tool in peptide mass spectrometry research.

  13. The effects of analyte mass and collision gases on ion beam formation in an inductively coupled plasma mass spectrometer

    Science.gov (United States)

    Larsen, Jessica J.; Edmund, Alisa J.; Farnsworth, Paul B.

    2016-11-01

    Planar laser induced fluorescence (PLIF) was used to evaluate the effect of matrix components on the formation and focusing of a Ba ion beam in a commercial inductively coupled plasma mass spectrometer. Cross sections of the ion beams were taken in the second vacuum stage, in front of the entrance to the mass analyzer. Under normal operating conditions, the addition of Pb shifted the position of the Ba ion beam to the right. PLIF was also used to evaluate the effect of a collision reaction interface (CRI) on Ca and Ba ion beams. A wider velocity distribution of ions and a decrease in overall intensity were observed for the CRI images. The fluorescence and mass spectrometer signals decreased with increased CRI flow rates. These effects were most obvious for Ca ions with He gas.

  14. A specialized isotope mass spectrometer for noninvasive diagnostics of Helicobacter pylori infection in human beings

    Science.gov (United States)

    Blashenkov, N. M.; Sheshenya, E. S.; Solov'ev, S. M.; Sachenko, V. D.; Gall, L. N.; Zarutskii, I. V.; Gall, N. R.

    2013-05-01

    A specialized isotope mass spectrometer for noninvasive diagnostics of Helicobacter pylori infection in human beings based on the carbon-13 isotope breath test has been designed and constructed. Important stages of the work included (i) calculating a low-aberration mass analyzer, (ii) manufacturing and testing special gas inlet system, and (iii) creating a small-size collector of ions. The proposed instrument ensures 13C/12C isotopic ratio measurement to within 1.7‰ (pro mille) accuracy, which corresponds to requirements for a diagnostic tool. Preliminary medical testing showed that the mass spectrometer is applicable to practical diagnostics. The instrument is also capable of measuring isotopic ratios of other light elements, including N, O, B (for BF2+ ions), Ar, Cl, and S.

  15. A High-Resolution Time-of-Flight Mass Spectrometer for Experiments with Ultracold Gases

    CERN Document Server

    Kraft, S D; Staanum, P; Fioretti, A; Lange, J; Wester, R; Weidemüller, M; Kraft, Stephan D.; Mikosch, Jochen; Staanum, Peter; Fioretti, Andrea; Lange, Joerg; Wester, Roland; Weidemueller, Matthias

    2005-01-01

    We have realized a high-resolution time-of-flight mass spectrometer combined with a magneto-optical trap. The spectrometer enables excellent optical access to the trapped atomic cloud using properly devised acceleration and deflection electrodes. The ions are extracted along a laser axis and deflected onto an off axis detector. The setup is applied to detect atoms and molecules photoassociated from ultracold atoms. The detection is based on resonance-enhanced multi-photon ionization. The versatile setup can easily be implemented in more complex experiments with ultracold atomic and molecular gases. Mass resolution up to $m/\\Delta m_{rms} = 1000$ at the mass of $^{133}$Cs is achieved.

  16. Mobile high-resolution time-of-flight mass spectrometer for in-situ analytics

    Energy Technology Data Exchange (ETDEWEB)

    Lang, Johannes; Ebert, Jens [II. Physikalisches Institut, JLU, Giessen (Germany); Dickel, Timo; Geissel, Hans; Plass, Wolfgang; Scheidenberger, Christoph [II. Physikalisches Institut, JLU, Giessen (Germany); GSI, Darmstadt (Germany)

    2011-07-01

    A compact multiple-reflection time-of-flight mass spectrometer (MR-TOF-MS) has been developed. For the first time it allows for mass measurements with a resolving power exceeding 100000 and sub ppm accuracy in a mobile device. Thus it allows to resolve isobars and enables to accurately determine the composition and structure of biomolecules. The MR-TOF-MS consists of an atmospheric pressure interface for DESI and REIMS, ion cooler, ion trap, time-of-flight analyzer, MCP detector and DAQ. Vacuum system components, power supplies as well as electronics are mounted together with the ion optical spectrometer parts on a single frame with a total volume of 0.8 m{sup 3}. Applications of the device within the AmbiProbe research program include in-situ mass spectrometry such as real-time tissue recognition in electrosurgery, identification of mycotoxins and analysis of soil samples for environmental studies.

  17. A High Resolution Orbitrap Mass Spectrometer for In-Situ Analysis in Planetary Science

    Science.gov (United States)

    Briois, C.; Thirkell, L.; Boukrara, A.; Lebreton, J. P.; Thissen, R.; Puget, P.; Cottin, H.; Grand, N.; Pennanech, C.; Zapf, P.; Szopa, C.; Carrasco, N.; Chapuis, C.; Bouabdellah, A.; Berthelier, J. J.; Engrand, C.; Makarov, A.

    2012-04-01

    Solar System exploration is dealing more and more with chemically complex matter, potentially associated with astrobiology or prebiotic questions, requiring optimized methods of analysis. Due to its ability to reveal quantitatively almost any chemical element, mass spectrometry has served as an invaluable scientific analytical instruments. Nevertheless the best mass resolution (M/deltaM) currently achieved by mass spectrometers in space is about 3000 at mass 28 (ROSINA's DFMS on board ESA's comet chaser Rosetta). This resolution allows separation of peaks for only a limited number of isobaric species (e.g. N2 / CO at 28 Da). Yet, purely electrostatic orbital traps in laboratory are showing mass resolution above 100 000 for m/z <= 400 [1, 2], that provides separation for each detected isobaric species. Therefore it opens new opportunity for molecular characterization, isotopic abundance evaluation, and more generally environmental characterization. Our French consortium of laboratories, in collaboration with ThermoFischer Scientific, is currently working on the adaptation of this type of mass spectrometer for space instrumentation. We present here this innovative concept of mass analyzer for space that is lightweight, uses DC voltages, and provides ultra high resolving power capabilities. A mass resolution of 140,000 at mass 56 has been recently achieved with our prototype.

  18. Penning trap mass measurements of $^{99-109}$Cd with the ISOLTRAP mass spectrometer, and implications for the rp process

    CERN Document Server

    Breitenfeldt, M; Beck, D; Blaum, K; George, S; Herfurth, F; Herlert, A; Kellerbauer, A G; Kluge, H-J; Kowalska, M; Lunney, D; Naimi, S; Neidherr, D; Schatz, H; Schwarz, S; Schweikhard, L

    2009-01-01

    Penning trap mass measurements on neutron-deficient Cd isotopes $^{99-109}$Cd have been performed with the ISOLTRAP mass spectrometer at ISOLDE/CERN, all with relative mass uncertainties below $3 \\times 10^{-8}$. A new mass evaluation has been performed. The mass of $^{99}$Cd has been determined for the first time which extends the region of accurately known mass values towards the doubly magic nucleus $^{100}$Sn. The implication of the results on the reaction path of the $rp$ process in stellar X-ray bursts is discussed. In particular, the uncertainty of the abundance and the overproduction created by the $rp$-process for the mass A = 99 is demonstrated by reducing the uncertainty of the proton-separation energy of $^{100}$In $S_{p}(^{100}$In) by a factor of 2.5.

  19. A Remote Laser-mass Spectrometer for Determination of Elemental Composition

    Science.gov (United States)

    Deyoung, R. J.; Situ, W.

    1993-01-01

    Determination of the elemental composition of lunar, asteroid, and planetary surfaces is a major concern for science and resource utilization of space. The science associated with the development of a satellite or lunar rover laser-mass spectrometer instrument is presented here. The instrument would include a pulsed laser with sufficient energy to create a plasma on a remote surface. Ions ejected from this plasma travel back to the spacecraft or rover, where they are analyzed by a time-of-flight mass spectrometer, giving the elemental and isotope composition. This concept is based on the LIMA-D instrument on board the former Soviet Union Phobos-88 spacecraft sent to Mars. A laser-mass spectrometer placed on a rover or satellite would substantially improve the data return over alternative techniques. The spatial resolution would be centimeters, and a complete mass spectrum could be achieved in one laser shot. An experiment is described that demonstrates these features. A 400 mj Nd:YAG laser is focused, to an intensity of 10(exp 11) w/sq cm, onto a Al, Ag, Cu, Ge, or lunar simulant target. A plasma forms from which ions are ejected. Some of these ions travel down an 18-m evacuated flight tube to a microchannel plate detector. Alternatively, the ions are captured by an ion trap where they are stored until pulsed into a 1-m time-of-flight mass spectrometer, giving the elemental composition of the remote surface. A television camera monitors the plasma plume shape, and a photodiode monitors the temporal plasma emission . With this system, ions of Al, Ag, Cu, Ge, and lunar simulant have been detected at 18 m. The mass spectrum from the ion trap and 1-m time-of-flight tube will be presented.

  20. Planar differential mobility spectrometer as a pre-filter for atmospheric pressure ionization mass spectrometry.

    Science.gov (United States)

    Schneider, Bradley B; Covey, Thomas R; Coy, Stephen L; Krylov, Evgeny V; Nazarov, Erkinjon G

    2010-12-01

    Ion filters based on planar DMS can be integrated with the inlet configuration of most mass spectrometers, and are able to enhance the quality of mass analysis and quantitative accuracy by reducing chemical noise, and by pre-separating ions of similar mass. This paper is the first in a series of three papers describing the optimization of DMS / MS instrumentation. In this paper the important physical parameters of a planar DMS-MS interface including analyzer geometry, analyzer coupling to a mass spectrometer, and transport gas flow control are considered. The goal is to optimize ion transmission and transport efficiency, provide optimal and adjustable resolution, and produce stable operation under conditions of high sample contamination. We discuss the principles of DMS separations and highlight the theoretical underpinnings. The main differences between planar and cylindrical geometries are presented, including a discussion of the advantages and disadvantages of RF ion focusing. In addition, we present a description of optimization of the frequency and amplitude of the DMS fields for resolution and ion transmission, and a discussion of the influence and importance of ion residence time in DMS. We have constructed a mass spectrometer interface for planar geometries that takes advantage of atmospheric pressure gas dynamic principles, rather than ion focusing, to minimize ion losses from diffusion in the analyzer and to maximize total ion transport into the mass spectrometer. A variety of experimental results has been obtained that illustrate the performance of this type of interface, including tests of resistance to high contamination levels, and the separation of stereoisomers. In a subsequent publication the control of the chemical interactions that drive the separation process of a DMS / MS system will be considered. In a third publication we describe novel electronics designed to provide the high voltages asymmetric waveform fields (SV) required for these

  1. Validation of a qualitative screening method for pesticides in fruits and vegetables by gas chromatography quadrupole-time of flight mass spectrometry with atmospheric pressure chemical ionization

    Energy Technology Data Exchange (ETDEWEB)

    Portolés, T. [Research Institute for Pesticides and Water, University Jaume I, 12071 Castellón (Spain); RIKILT Institute of Food Safety, Wageningen University and Research Centre, Akkermaalsbos 2, 6708 WB Wageningen (Netherlands); Mol, J.G.J. [RIKILT Institute of Food Safety, Wageningen University and Research Centre, Akkermaalsbos 2, 6708 WB Wageningen (Netherlands); Sancho, J.V.; López, Francisco J. [Research Institute for Pesticides and Water, University Jaume I, 12071 Castellón (Spain); Hernández, F., E-mail: hernandf@uji.es [Research Institute for Pesticides and Water, University Jaume I, 12071 Castellón (Spain)

    2014-08-01

    Highlights: • Applicability of GC-(APCI)QTOF MS as new tool for wide-scope screening of pesticides in fruits and vegetables demonstrated. • Validation of screening method according to SANCO/12571/2013. • Detection of the pesticides based on the presence of M+·/MH+ in most cases. • Screening detection limit 0.01 mg kg{sup −1} for 77% of the pesticides investigated. • Successful identification at 0.01 mg kg{sup −1} for 70% of the pesticides/matrix combinations. - Abstract: A wide-scope screening method was developed for the detection of pesticides in fruit and vegetables. The method was based on gas chromatography coupled to a hybrid quadrupole time-of-flight mass spectrometer with an atmospheric pressure chemical ionization source (GC-(APCI)QTOF MS). A non-target acquisition was performed through two alternating scan events: one at low collision energy and another at a higher collision energy ramp (MS{sup E}). In this way, both protonated molecule and/or molecular ion together with fragment ions were obtained in a single run. Validation was performed according to SANCO/12571/2013 by analysing 20 samples (10 different commodities in duplicate), fortified with a test set of 132 pesticides at 0.01, 0.05 and 0.20 mg kg{sup −1}. For screening, the detection was based on one diagnostic ion (in most cases the protonated molecule). Overall, at the 0.01 mg kg{sup −1} level, 89% of the 2620 fortifications made were detected. The screening detection limit for individual pesticides was 0.01 mg kg{sup −1} for 77% of the pesticides investigated. The possibilities for identification according to the SANCO criteria, requiring two ions with a mass accuracy ≤±5 ppm and an ion-ratio deviation ≤±30%, were investigated. At the 0.01 mg kg{sup −1} level, identification was possible for 70% of the pesticides detected during screening. This increased to 87% and 93% at the 0.05 and 0.20 mg kg{sup −1} level, respectively. Insufficient sensitivity for the second

  2. Paired-ion electrospray ionization--triple quadrupole tandem mass spectrometry for quantification of anionic surfactants in waters.

    Science.gov (United States)

    Santos, Inês C; Guo, Hongyue; Mesquita, Raquel B R; Rangel, António O S S; Armstrong, Daniel W; Schug, Kevin A

    2015-10-01

    A new paired ion electrospray ionization tandem mass spectrometry method for determination of anionic surfactants in water samples was developed. In this method, dicationic ion-pairing reagents were complexed with monoanionic analytes to facilitate analyte detection in positive mode electrospray ionization - mass spectrometry. Single ion monitoring and selected reaction monitoring on a triple quadrupole instrument were performed and compared. Four dicationic reagents were tested for the determination of perfluorooctanoic acid (PFOA), perfluorooctane sulfonate (PFOS), sodium dodecyl sulfate (SDS), dodecylbenzene sulfonic acid (DBS), and stearic acid (SA), among other common anions. The obtained limits of detection were compared with those from previous literature. Solid phase extraction using a C18 cartridge was performed in order to eliminate matrix interferences. A literature review was compiled for the methods published between 2010 and 2015 for determination of anionic surfactants. The optimized method was more sensitive than previously developed methods with LOD values of 2.35, 35.4, 37.0, 1.68, and 0.675 pg for SDS, SA, DBS, PFOS, and PFOA, respectively. The developed method was effectively applied for the determination of anionic surfactants in different water samples such as bottled drinking water, cooking water, tap water, and wastewater.

  3. Shotgun lipidomics on a LTQ Orbitrap mass spectrometer by successive switching between acquisition polarity modes

    DEFF Research Database (Denmark)

    Schuhmann, K.; Almeida, R.; Baumert, M.

    2012-01-01

    polarity, and therefore it is beneficial to analyze lipid mixtures in both positive and negative modes. Hybrid LTQ Orbitrap mass spectrometers are widely applied in topdown lipidomics; however, rapid polarity switching was previously unfeasible because of the severe and immediate degradation of mass...... accuracy. Here, we report on a method to rapidly acquire high-resolution spectra in both polarity modes with sub-ppm mass accuracy and demonstrate that it not only simplifies and accelerates shotgun lipidomics analyses but also improves the lipidome coverage because more lipid classes and more individual...

  4. Methods for SWATH™: Data Independent Acquisition on TripleTOF Mass Spectrometers.

    Science.gov (United States)

    Holewinski, Ronald J; Parker, Sarah J; Matlock, Andrea D; Venkatraman, Vidya; Van Eyk, Jennifer E

    2016-01-01

    Data independent acquisition (DIA also termed SWATH) is an emerging technology in the field of mass spectrometry based proteomics. Although the concept of DIA has been around for over a decade, the recent advancements, in particular the speed of acquisition, of mass analyzers have pushed the technique into the spotlight and allowed for high-quality DIA data to be routinely acquired by proteomics labs. In this chapter we will discuss the protocols used for DIA acquisition using the Sciex TripleTOF mass spectrometers and data analysis using the Sciex processing software.

  5. A Dual Source Ion Trap Mass Spectrometer for the Mars Organic Molecule Analyzer of ExoMars 2018

    Science.gov (United States)

    Brickerhoff, William B.; vanAmerom, F. H. W.; Danell, R. M.; Arevalo, R.; Atanassova, M.; Hovmand, L.; Mahaffy, P. R.; Cotter, R. J.

    2011-01-01

    We present details on the objectives, requirements, design and operational approach of the core mass spectrometer of the Mars Organic Molecule Analyzer (MOMA) investigation on the 2018 ExoMars mission. The MOMA mass spectrometer enables the investigation to fulfill its objective of analyzing the chemical composition of organic compounds in solid samples obtained from the near surface of Mars. Two methods of ionization are realized, associated with different modes of MOMA operation, in a single compact ion trap mass spectrometer. The stringent mass and power constraints of the mission have led to features such as low voltage and low frequency RF operation [1] and pulse counting detection.

  6. Mass measurements on neutron-deficient Sr and neutron-rich Sn isotopes with the ISOLTRAP mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Sikler, G. [MPI fuer Kernphysik, Saupfercheckweg 1, 69117 Heidelberg (Germany) and TRIUMF, 4004 Wesbrook Mall, Vancouver BC, V6T 2A3 (Canada)]. E-mail: g.sikler@mpi-hd.mpg.de; Audi, G. [CSNSM-IN2P3-CNRS, Batiment 108, 91405 Orsay-Campus (France); Beck, D. [GSI, Planckstr. 1, 64291 Darmstadt (Germany); Blaum, K. [Johannes Gutenberg-Universitaet Mainz, Staudingerweg 7, 55128 Mainz (Germany); Bollen, G. [NSCL, Michigan State University, East Lansing, MI 48824-1321 (United States); Herfurth, F. [GSI, Planckstr. 1, 64291 Darmstadt (Germany); Kellerbauer, A. [CERN, 1211 Geneva 23 (Switzerland); Kluge, H.-J. [GSI, Planckstr. 1, 64291 Darmstadt (Germany); Lunney, D. [CSNSM-IN2P3-CNRS, Batiment 108, 91405 Orsay-Campus (France); Oinonen, M. [Helsinki Institute of Physics, P.O. Box 64, 00014 University of Helsinki (Finland); Scheidenberger, C. [GSI, Planckstr. 1, 64291 Darmstadt (Germany); Schwarz, S. [NSCL, Michigan State University, East Lansing, MI 48824-1321 (United States); Szerypo, J. [LMU Muenchen, Am Coulombwall 1, 85748 Garching (Germany)

    2005-12-26

    The atomic masses of {sup 76,77,80,81,86,88}Sr and {sup 124,129,130,131,132}Sn were measured by means of the Penning trap mass spectrometer ISOLTRAP at ISOLDE/CERN. {sup 76}Sr is now the heaviest N=Z nucleus for which the mass is measured to a precision better than 35 keV. For the tin isotopes in the close vicinity of the doubly magic nucleus {sup 132}Sn, mass uncertainties below 20 keV were achieved. An atomic mass evaluation was carried out taking other experimental mass values into account by performing a least-squares adjustment. Some discrepancies between older experimental values and the ones reported here emerged and were resolved. The results of the new adjustment and their impact will be presented.

  7. Mass measurements on neutron-deficient Sr and neutron-rich Sn isotopes with the ISOLTRAP mass spectrometer

    CERN Document Server

    Sikler, G; Beck, D; Blaum, K; Bollen, G; Herfurth, F; Kellerbauer, A G; Kluge, H J; Lunney, M D; Oinonen, M; Scheidenberger, C; Schwarz, S; Szerypo, J

    2005-01-01

    The atomic masses of $^{76,77,80,81,86,88}$Sr and $^{124,129,130,131,132}$Sn were measured by means of the Penning trap mass spectrometer ISOLTRAP at ISOLDE/CERN. $^{76}$Sr is now the heaviest N=Z nucleus for which the mass is measured to a precision better than 35 keV. For the tin isotopes in the close vicinity of the doubly magic nucleus $^{132}$Sn, mass uncertainties below 20 keV were achieved. An atomic mass evaluation was carried out taking other experimental mass values into account by performing a least-squares adjustment. Some discrepancies between older experimental values and the ones reported here emerged and were resolved. The results of the new adjustment and their impact will be presented.

  8. Characterization and quantitative analysis of surfactants in textile wastewater by liquid chromatography/quadrupole-time-of-flight mass spectrometry.

    Science.gov (United States)

    González, Susana; Petrović, Mira; Radetic, Maja; Jovancic, Petar; Ilic, Vesna; Barceló, Damià

    2008-05-01

    A method based on the application of ultra-performance liquid chromatography (UPLC) coupled to hybrid quadrupole-time-of-flight mass spectrometry (QqTOF-MS) with an electrospray (ESI) interface has been developed for the screening and confirmation of several anionic and non-ionic surfactants: linear alkylbenzenesulfonates (LAS), alkylsulfate (AS), alkylethersulfate (AES), dihexyl sulfosuccinate (DHSS), alcohol ethoxylates (AEOs), coconut diethanolamide (CDEA), nonylphenol ethoxylates (NPEOs), and their degradation products (nonylphenol carboxylate (NPEC), octylphenol carboxylate (OPEC), 4-nonylphenol (NP), 4-octylphenol (OP) and NPEO sulfate (NPEO-SO4). The developed methodology permits reliable quantification combined with a high accuracy confirmation based on the accurate mass of the (de)protonated molecules in the TOFMS mode. For further confirmation of the identity of the detected compounds the QqTOF mode was used. Accurate masses of product ions obtained by performing collision-induced dissociation (CID) of the (de)protonated molecules of parent compounds were matched with the ions obtained for a standard solution. The method was applied for the quantitative analysis and high accuracy confirmation of surfactants in complex mixtures in effluents from the textile industry. Positive identification of the target compounds was based on accurate mass measurement of the base peak, at least one product ion and the LC retention time of the analyte compared with that of a standard. The most frequently surfactants found in these textile effluents were NPEO and NPEO-SO4 in concentrations ranging from 0.93 to 5.68 mg/L for NPEO and 0.06 to 4.30 mg/L for NPEO-SO4. AEOs were also identified.

  9. The Multiplexed Chemical Kinetic Photoionization Mass Spectrometer: A New Approach To Isomer-resolved Chemical Kinetics

    Energy Technology Data Exchange (ETDEWEB)

    Osborne, David L.; Zou, Peng; Johnsen, Howard; Hayden, Carl C.; Taatjes, Craig A.; Knyazev, Vadim D.; North, Simon W.; Peterka, Darcy S.; Ahmed, Musahid; Leone, Stephen R.

    2008-08-28

    We have developed a multiplexed time- and photon-energy?resolved photoionizationmass spectrometer for the study of the kinetics and isomeric product branching of gasphase, neutral chemical reactions. The instrument utilizes a side-sampled flow tubereactor, continuously tunable synchrotron radiation for photoionization, a multi-massdouble-focusing mass spectrometer with 100percent duty cycle, and a time- and positionsensitive detector for single ion counting. This approach enables multiplexed, universal detection of molecules with high sensitivity and selectivity. In addition to measurement of rate coefficients as a function of temperature and pressure, different structural isomers can be distinguished based on their photoionization efficiency curves, providing a more detailed probe of reaction mechanisms. The multiplexed 3-dimensional data structure (intensity as a function of molecular mass, reaction time, and photoionization energy) provides insights that might not be available in serial acquisition, as well as additional constraints on data interpretation.

  10. Preserving the Sequence of a Biopolymer's Monomers as They Enter an Electrospray Mass Spectrometer

    Science.gov (United States)

    Maulbetsch, William; Wiener, Benjamin; Poole, William; Bush, Joseph; Stein, Derek

    2016-11-01

    This paper investigates how faithfully an electrospray mass spectrometer reports the order of monomers of a single biopolymer in the context of two sequencing strategies. We develop a simplified one-dimensional theoretical model of the dynamics of Brownian particles in the Taylor cone of an electropray source, where free monomers drift towards the apex in an elongational force gradient. The likelihood that neighboring particles will invert their order decreases near the apex because the strength of the force gradient increases. Neighboring monomers on a stretched biopolymer should be cleaved by photofragmentation within about 3 nm of the apex if they are to enter the mass spectrometer in sequence with 95% probability under typical experimental conditions. Alternatively, if the monomers are cleaved processively at milliseconds-long intervals by an enzyme, their sequence will be faithfully reported with 95% confidence if the enzyme is within about 117 nm of the apex.

  11. Rapid identification of polymer additives by atmospheric solid analysis probe with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Du, Zhenxia; Zhang, Yun; Li, Ailin; Lv, Surong

    2014-10-15

    A method using an atmospheric solid analysis probe (ASAP) combined with quadrupole time-of-flight mass spectrometry (QTOFMS) assisted by a pre-built MS library was found to be efficient in fast and direct analysis of additives for polymers. By this method, sample pretreatment could be eliminated from the additives identification process. Some crucial parameters, such as desolvation gas temperature, corona current, sample cone voltage and collision energy, should be optimized. A MS library of 100 polymer additives, including phenols (Irganox 1010, Irganox 1076), hydroxyl phenyl benzotriazole derivatives (Tinuvin 326, Tinuvin 327, Tinuvin 328), hindered amines (Tinuvin 944, Tinuvin 770) and plasticizers, was built based on the optimized conditions. To verify the application of the MS library, the ASAP-QTOFMS method was applied to identify complex additives, a simulated polypropylene (PP) sample and a real polymethylmethacrylate (PMMA) sample purchased from a local market. By searching the exact mass, and comparing the MS and MS/MS spectra of samples with standards in the MS library, complex additives such as Irganox GX 2921, as well as additives in PP and PMMA samples, could be identified quickly and easily. The determination of mass accuracy increased the confidence of peak identification as well. Moreover, the results also provided information of the characterization for PP and PMMA polymers. A rapid identification method has been developed for polymer additives by ASAP-QTOFMS. A MS library of 100 polymer additives was built by this method. Using ASAP-QTOFMS assisted by the pre-built MS library, polymer additives can be quickly identified. This method was found to be a promising tool in the rapid analysis of additives in polymers and polymer matrices. Copyright © 2014 John Wiley & Sons, Ltd.

  12. Conformational ordering of biomolecules in the gas phase: nitrogen collision cross sections measured on a prototype high resolution drift tube ion mobility-mass spectrometer.

    Science.gov (United States)

    May, Jody C; Goodwin, Cody R; Lareau, Nichole M; Leaptrot, Katrina L; Morris, Caleb B; Kurulugama, Ruwan T; Mordehai, Alex; Klein, Christian; Barry, William; Darland, Ed; Overney, Gregor; Imatani, Kenneth; Stafford, George C; Fjeldsted, John C; McLean, John A

    2014-02-18

    Ion mobility-mass spectrometry measurements which describe the gas-phase scaling of molecular size and mass are of both fundamental and pragmatic utility. Fundamentally, such measurements expand our understanding of intrinsic intramolecular folding forces in the absence of solvent. Practically, reproducible transport properties, such as gas-phase collision cross-section (CCS), are analytically useful metrics for identification and characterization purposes. Here, we report 594 CCS values obtained in nitrogen drift gas on an electrostatic drift tube ion mobility-mass spectrometry (IM-MS) instrument. The instrument platform is a newly developed prototype incorporating a uniform-field drift tube bracketed by electrodynamic ion funnels and coupled to a high resolution quadrupole time-of-flight mass spectrometer. The CCS values reported here are of high experimental precision (±0.5% or better) and represent four chemically distinct classes of molecules (quaternary ammonium salts, lipids, peptides, and carbohydrates), which enables structural comparisons to be made between molecules of different chemical compositions for the rapid "omni-omic" characterization of complex biological samples. Comparisons made between helium and nitrogen-derived CCS measurements demonstrate that nitrogen CCS values are systematically larger than helium values; however, general separation trends between chemical classes are retained regardless of the drift gas. These results underscore that, for the highest CCS accuracy, care must be exercised when utilizing helium-derived CCS values to calibrate measurements obtained in nitrogen, as is the common practice in the field.

  13. Development of a linear ion trap/orthogonal-time-of-flight mass spectrometer for time-dependent observation of product ions by ultraviolet photodissociation of peptide ions.

    Science.gov (United States)

    Kim, Tae-Young; Schwartz, Jae C; Reilly, James P

    2009-11-01

    A hybrid linear ion trap/orthogonal time-of-flight (TOF) mass spectrometer has been developed to observe time-dependent vacuum ultraviolet photodissociation product ions. In this apparatus, a reflectron TOF mass analyzer is orthogonally interfaced to an LTQ using rf-only octopole and dc quadrupole ion guides. Precursor ions are generated by electrospray ionization and isolated in the ion trap. Subsequently they are directed to the TOF source where photodissociation occurs and product ions are extracted for mass analysis. To detect photodissociation product ions having axially divergent trajectories, a large rectangular detector is utilized. With variation of the time between photodissociation and orthogonal extraction in the TOF source, product ions formed over a range of times after photoexcitation can be sampled. Time-dependent observation of product ions following 157 nm photodissociation of a singly charged tryptic peptide ion (NWDAGFGR) showed that prompt photofragment ions (x- and v-type ions) dominate the tandem mass spectrum up to 1 micros after the laser shot, but the intensities of low energy thermal fragment ions (y-type ions) become comparable several microseconds later. Different proton mobilization time scales were observed for arginine- and lysine-terminated tryptic peptides.

  14. Simultaneous determination of 23 flavor additives in tobacco products using gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Zhang, Yi; Wang, Xiujuan; Li, Li; Li, Weiqing; Zhang, Feng; Du, Tianxin; Chu, Xiaogang

    2013-09-06

    A method based on gas chromatography coupled to triple quadrupole tandem mass spectrometry (GC-QqQ MS/MS) was developed for the determination of 23 widely used flavor additives in tobacco products in this paper. The MS/MS fragmentation pathway of the cinnamic esters additives was illustrated. The new analytical method was defined based on two main axes, ultrasonic solvent extraction procedure with dichloromethane and analyte detection performed by GC-QqQ MS/MS in electron impact mode. The excellent selectivity and sensitivity achieved in multiple reactions monitoring (MRM) mode allowed satisfactory confirmation and quantitation for the tobacco flavor additives. The linear range of the 23 flavor additives is 0.2-500.0μg/L with good correlation coefficients (r(2)>0.9963). The limits of detection (LODs) and limits of quantitation (LOQs) of these compounds were in the range 0.1-2.0μg/L and 0.4-6.0μg/kg, respectively. The average recoveries at three spiked levels (LOQ, 2LOQ, 4LOQ) were all in the range 62.1-93.8% with RSDs (n=6) lower than 7.8%. The method of GC-QqQ MS/MS developed in this study was initially applied to the research of flavor additives in 12 retail cigarette samples and proved to be accurate, sensitive, convenient and practical. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Qualitative identification of dibenzoylmethane in licorice root (Glycyrrhiza glabra) using gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Mancia, Marisela D; Reid, Michelle E; DuBose, Evan S; Campbell, James A; Jackson, Kimberly M

    2014-01-01

    Licorice root (Glycyrrhiza glabra), an herbal Chinese medicine, has shown medicinal uses in therapeutics and cancer prevention. Dibenzoylmethane (DBM; 1, 3-diphenyl-1, 3-propadinedione), a small beta-diketone, has been reported to be a minor constituent of licorice and a known deregulator of the human prostate cancer cell cycle. Characterization of the phytochemical profiles of licorice root forms including commercially available DBM will advance our search in identifying novel reagents for prostate cancer therapeutics. Gas chromatography- triple quadrupole-mass spectrometric analysis was used for detecting DBM in licorice root extracts. DBM and all licorice forms exhibited a component with a retention time of 14.5 minutes. The major fragment ions detected were at m/z 77, 105, 147, 223 and 224 at the identified retention time by selected reaction monitoring/SRM. These data confirm the presence of DBM from its natural source (G. glabra), and the GC-MS/SRM method helps in the identification of this minor component in a complex biological matrix.

  16. Trace determination of 13 haloacetamides in drinking water using liquid chromatography triple quadrupole mass spectrometry with atmospheric pressure chemical ionization.

    Science.gov (United States)

    Chu, Wenhai; Gao, Naiyun; Yin, Daqiang; Krasner, Stuart W; Templeton, Michael R

    2012-04-27

    The haloacetamides (HAcAms) are disinfection by-products (DBPs) in drinking water which are currently receiving increased scientific attention due to their elevated toxicity relative to regulated disinfection by-products. A simultaneous determination method of 13 HAcAms, combining solid-phase extraction (SPE) enrichment, liquid chromatographic (LC) separation, and triple quadrupole mass spectrometry (tqMS) detection with atmospheric pressure chemical ionization (APCI) using selective reaction monitoring in positive mode, was developed to measure HAcAms, including chlorinated, brominated, and iodinated analogs. Ammonium chloride and Oasis HLB were selected as the dechlorinating reagent and polymeric SPE sorbent of HAcAm samples. The used tqMS apparatus showed higher sensitivity for the studied HAcAms in the APCI mode than electrospray ionization. 13 HAcAms were separated by LC in 9.0 min, and the detection limits ranged from 7.6 to 19.7 ng/L. The SPE-LC/tqMS method was successfully applied to quantify 13 HAcAms in drinking water samples for the first time, and first indentified tribromoacetamide and chloroiodoacetamide as DBPs in drinking water.

  17. Profiling the Metabolism of Astragaloside IV by Ultra Performance Liquid Chromatography Coupled with Quadrupole/Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xu-Dong Cheng

    2014-11-01

    Full Text Available Astragaloside IV is a compound isolated from the Traditional Chinese Medicine Astragalus membranaceus, that has been reported to have bioactivities against cardiovascular disease and kidney disease. There is limited information on the metabolism of astragaloside IV, which impedes comprehension of its biological actions and pharmacology. In the present study, an ultra-performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS-based approach was developed to profile the metabolites of astragaloside IV in rat plasma, bile, urine and feces samples. Twenty-two major metabolites were detected. The major components found in plasma, bile, urine and feces included the parent chemical and phases I and II metabolites. The major metabolic reactions of astragaloside IV were hydrolysis, glucuronidation, sulfation and dehydrogenation. These results will help to improve understanding the metabolism and reveal the biotransformation profiling of astragaloside IV in vivo. The metabolic information obtained from our study will guide studies into the pharmacological activity and clinical safety of astragaloside IV.

  18. Quantification of steroidal alkaloids in Buxus papillosa using electrospray ionization liquid chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Musharraf, Syed Ghulam; Goher, Madiha; Zareena, Bibi

    2015-08-01

    Buxus papillosa is one of the most extensively studied species of the genus Buxus known to possess steroidal alkaloids which can be used for assessing the various pharmacological activities of this plant. This paper describes the liquid chromatography-electrospray ionization triple quadrupole mass spectrometry (LC-ESI-QQQ-MS) method for the quantification of six steroidal alkaloids as chemical markers in the extracts of leaves, roots and stems of B. papillosa. Quantitative MS/MS analysis was carried out by optimization of the most sensitive transition for each analyte. This has yielded detection and quantification limits of 0.486-8.08 ng/mL and 1.473-24.268 ng/mL, respectively for all analytes. Linearity of response was also achieved and the regression coefficient found to be >0.99 for all analyzed compounds. The newly developed MRM (Multiple Reaction Monitoring) method showed excellent sensitivity for the quantification of steroidal alkaloids within 15 min run time. This paper describes the application of LC-QQQ-MS technique for steroidal alkaloids analysis in plant samples.

  19. Rapid and Accurate U-Th Dating of Ancient Carbonates using Inductively Coupled Plasma-Quadrupole Mass Spectrometry

    Science.gov (United States)

    Douville, Eric; Sallé, Eline; Frank, Norbert; Eisele, Markus; Pons-Branchu, Edwige; Ayrault, Sophie

    2010-05-01

    Here, the potential for rapid and accurate U-Th dating technique of marine aragonite skeletons (deep-sea corals, Lophelia pertusa) and secondary calcite deposits (speleothems and stalagmites) has been explored using inductively-coupled plasma-quadrupole mass spectrometry (ICP-QMS). The analytical procedure includes a largely simplified chemical separation technique for uranium (U) and thorium (Th) using UTEVA resin. The developed technique permits simultaneous quantification of uranium [238U] and thorium [232Th] concentrations and their respective isotopic composition, required for U-series disequilibrium dating. Up to 50 U-Th dates per day can be achieved through ICP-QMS with 234U and 230Th reproducibility (2sigma) of 3-4 permil and 1 percent, respectively. The high sensitivity (> 300 000 cps/ppb) together with low background (Porcupine Seabight (MD01-2463G, Mound Thérèse), indicating a purely interglacial growth of deep-water corals on so-called carbonate mounds over several climate cycles.

  20. Nucleation phenomena during molecular beam epitaxy of GaN observed by line-of-sight quadrupole mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Koblmueller, G.; Averbeck, R.; Riechert, H. [Infineon Technologies AG, Corporate Research Photonics, Otto-Hahn-Ring 6, 81739 Munich (Germany); Pongratz, P. [Vienna University of Technology, Institute of Solid State Physics, Wiedner Hauptstrasse 8-10, 1040 Vienna (Austria)

    2002-12-16

    We investigate nucleation and growth phenomena during molecular beam epitaxy of GaN on sapphire, 6H-SiC and GaN templates using in situ line-of-sight quadrupole mass spectrometry. Moreover, this method allows the quantitative study of nucleation phenomena by monitoring desorption processes. Heteroepitaxial growth of GaN on sapphire and 6H-SiC faces a high energy barrier to nucleation giving rise to a substantial Ga desorption during the initial phase of nucleation. The amount of initial Ga desorption in heteroepitaxy is independent of the chosen substrate material and is as high as 8 {+-} 1.5 nm equivalent GaN thickness. Once critical-sized islands have nucleated they grow three-dimensional (3D) leading to a quadratic increase of the GaN coverage and finally to a steady growth rate after coalescence, as also determined by Rutherford backscattering and atomic force microscopy. In contrast, homoepitaxy on Ga- and N-face GaN templates is distinguished by immediate nucleation. (Abstract Copyright [2002], Wiley Periodicals, Inc.)

  1. Determination of parabens in environmental solid samples by ultrasonic-assisted extraction and liquid chromatography with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Núñez, L; Tadeo, J L; García-Valcárcel, A I; Turiel, E

    2008-12-19

    Analysis of various p-hydroxybenzoic esters (methyl, ethyl, isopropyl, propyl, benzyl, and butylparaben) in environmental solid samples was carried out by sonication-assisted extraction in small columns (SAESC) followed by liquid chromatography with triple quadrupole mass spectrometry (MS/MS). Solid samples were placed in small glass columns and extraction performed assisted by sonication in two consecutive steps of 15 min using acetonitrile as extraction solvent. Sample extracts were evaporated under nitrogen stream to 1 ml and analysed by LC-MS/MS. Satisfactory recoveries were obtained ranging from 83% to 110% depending on the analyte. Good limits of quantification (LOQs), between 0.11 and 0.49 ng g(-1) were obtained for LC-MS/MS, making this technique suitable for the determination of parabens in environmental solid samples, particularly at trace level. The developed method was applied to the determination of target analytes in different types of soil and sediments, finding levels between LOD and 6.35 ng g(-1).

  2. [Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry].

    Science.gov (United States)

    Liu, Xiaoqin; Tong, Ling; Meng, Wenting; Sun, Guoxiang

    2015-08-01

    A method was established for the simultaneous determination of 99 pesticide residues with combination of solid-phase extraction technique ( SPE) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS). The sample was extracted with ethyl acetate, and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0.001-0.25 mg/L, with correlation coefficients (r2) > 0.99. The limits of quantification (LOQs) were between 0.001-0.050 mg/kg. The recoveries were between 66.7% and 128.0% with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg/kg. This method has been applied to determine thirteen batches of commercially available samples, chlorpyriphos-ethyl and p,p'-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate, reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.

  3. Metabolite Analysis of Toosendanin by an Ultra-High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry Technique

    Directory of Open Access Journals (Sweden)

    Na Li

    2013-09-01

    Full Text Available Toosendanin is the major bioactive component of Melia toosendan Sieb. et Zucc., which is traditionally used for treatment of abdominal pain and as an insecticide. Previous studies reported that toosendanin possesses hepatotoxicity, but the mechanism remains unknown. Its bioavailability in rats is low, which indicates the hepatotoxicity might be induced by its metabolites. In this connection, in the current study, we examined the metabolites obtained by incubating toosendanin with human live microsomes, and then six of these metabolites (M1–M6 were identified for the first time by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF/MS. Further analysis on the MS spectra showed M1, M2, and M3 are oxidative products and M6 is a dehydrogenation product, while M4 and M5 are oxidative and dehydrogenation products of toosendanin. Moreover, their possible structures were deduced from the MS/MS spectral features. Quantitative analysis demonstrated that M1-M5 levels rapidly increased and reached a plateau at 30 min, while M6 rapidly reached a maximal level at 20 min and then decreased slowly afterwards. These findings have provided valuable data not only for understanding the metabolic fate of toosendanin in liver microsomes, but also for elucidating the possible molecular mechanism of its hepatotoxicity.

  4. Determination of polycyclic aromatic hydrocarbons in soy isoflavone nutraceutical products by gas chromatography coupled to triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Ruiz-Delgado, Ana; Martínez-Domínguez, Gerardo; Romero-González, Roberto; López-Ruiz, Rosalía; Frenich, Antonia Garrido

    2016-02-01

    Thirteen polycyclic aromatic hydrocarbons have been determined in soy-based nutraceutical products. First, an optimization of extraction procedure was performed, and a solid-liquid extraction assisted by sonication and a dilute and shoot procedure were compared, selecting the dilute and shoot approach for the extraction of target compounds, utilizing a mixture of acetone/n-hexane (1:1 v/v) as extractant solvent. After this, a clean-up step was needed bearing in mind the complexity of these matrices. Dispersive solid-phase extraction, using a mixture of C18 and Zr-Sep+ (25 mg/mL each) was used. The separation was achieved by gas chromatography and detection with triple quadrupole tandem mass spectrometry. For quantification purposes, matrix-matched calibration was used. The validation was applied at three concentration levels (20, 100 and 250 μg/kg), obtaining recoveries between 70 and 120% and precision values equal to or lower than 23%. Limits of detection and quantification were below 8 and 20 μg/kg, respectively. The method was applied in 11 samples, detecting five polycyclic aromatic hydrocarbons at concentrations ranging from 4.1 to 18.5 μg/kg.

  5. Determination of polychlorinated biphenyls in ambient air by gas chromatography coupled to triple quadrupole tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinez Ocana, Rosa; Mena Granero, Angela; Egea Gonzalez, Francisco J.; Garrido Frenich, Antonia; Martinez Vidal, Jose L.; Plaza Bolanos, Patricia [University of Almeria, Department of Analytical Chemistry, Almeria (Spain)

    2008-03-15

    A multiresidue method for determining 22 polychlorinated biphenyls (PCBs) in air has been developed and validated by gas chromatography (GC) coupled to tandem mass spectrometry (MS/MS) using a triple quadrupole analyzer (QqQ). The method was validated in terms of both steps of sampling and analysis. The sampling method, which is based on active sampling using polyurethane foam (PUF) as adsorbent, was validated by generating standard atmospheres. The retention capacity of this sampling sorbent allows up to 5 m{sup 3} of air to be sampled without any breakthrough for most compounds. Two solvent extraction methods were compared: sonication and Soxhlet extraction with a mixture of n-hexane:diethyl ether (95:5 v/v). Both extraction methods yielded similar results, but the first one required less solvent and time. The method exhibited good accuracy (80.3-99.8%), precision (2.2-15.2%) and lower limits that allowed quantification and confirmation at levels as low as 0.008 ng/m{sup 3}. Finally, the method was applied to the analysis of PCBs in the air in areas near to a municipal solid-waste landfill and directly above the refuse in the landfill, where it indicated the presence of some of the target compounds. (orig.)

  6. TRIGA-TRAP: A penning trap mass spectrometer at the research reactor TRIGA Mainz

    Energy Technology Data Exchange (ETDEWEB)

    Smorra, Christian [Physikalisches Institut, Universitaet Heidelberg (Germany); Institut fuer Kernchemie, Universitaet Mainz (Germany); Blaum, Klaus [Physikalisches Institut, Universitaet Heidelberg (Germany); Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany); Block, Michael; Herfurth, Frank [GSI, Helmholtzzentrum fuer Schwerionenforschung GmbH, Darmstadt (Germany); Eberhardt, Klaus [Institut fuer Kernchemie, Universitaet Mainz (Germany); Eibach, Martin; Ketelaer, Jens; Ketter, Jochen; Knuth, Konstantin; Repp, Julia [Institut fuer Physik, Universitaet Mainz (Germany); Nagy, Szilard [Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany)

    2009-07-01

    Nuclear masses represent the binding energies and, therefore, the sum of all interactions in the nucleus. They provide an important input parameter to nuclear structure models. Presently, a tremendous interest in masses of very exotic neutron-rich nuclides exists to support theoretical models for the nucleosynthesis via the rapid neutron capture process. The research reactor TRIGA Mainz provides access to a large variety of neutron-rich nuclides produced by thermal-neutron induced fission of an actinide target. The double-Penning trap mass spectrometer TRIGA-TRAP will perform high-precision mass measurements in this region of the nuclear chart as well as on actinides from uranium to californium. It also serves as a test facility for the development of new techniques that will be implemented in future facilities like MATS at FAIR (GSI, Darmstadt). The layout of TRIGA-TRAP as well as recent mass measurements are presented.

  7. A miniature laser ablation time-of-flight mass spectrometer for in situ planetary exploration

    Science.gov (United States)

    Rohner, Urs; Whitby, James A.; Wurz, Peter

    2003-12-01

    We report the development and testing of a miniature mass spectrometer and ion source intended to be deployed on an airless planetary surface to measure the elemental and isotopic composition of rocks and soils. Our design concentrates at this stage on the proposed BepiColombo mission to the planet Mercury. The mass analyser is an axially symmetric reflectron time-of-flight design. The ion source utilizes a laser induced plasma, which is directly coupled into the mass analyser. Laser ablation gives high spatial resolution, and avoids the need for sample preparation. Our prototype instrument has a demonstrated mass resolution m/Dgrm (FWHM) in excess of 600 and a predicted dynamic range of better than four orders of magnitude. Isotopic fractionation effects are found to be minor. We estimate that a flight instrument would have a mass of 500 g (including all electronics), a volume of 650 cm3 and could operate on 3 W power.

  8. A fragmentation study of kaempferol using electrospray quadrupole time-of-flight mass spectrometry at high mass resolution

    Science.gov (United States)

    March, Raymond E.; Miao, Xiu-Sheng

    2004-02-01

    A mass spectrometric method based on the combined use of electrospray ionization, collision-induced dissociation and tandem mass spectrometry at high mass resolution has been applied to an investigation of the structural characterization of protonated and deprotonated kaempferol (3,5,7,4'-tetrahydroxyflavone). Low-energy product ion mass spectra of [M+H]+ ions showed simple fragmentations of the C ring that permitted characterization of the substituents in the A and B rings. In addition, four rearrangement reactions accompanied by losses of C2H2O, CHO[radical sign], CO, and H2O were observed. Low-energy product ion mass spectra of [M-H]- ions showed only four rearrangement reactions accompanied by losses of OH[radical sign], CO, CH2O, and C2H2O. The use of elevated cone voltages permitted observation of product ion mass spectra of selected primary and secondary fragment ions so that each fragment ion reported was observed as a direct product of its immediate precursor ion. Product ion mass spectra examined at high mass resolution allowed unambiguous determination of the elemental composition of fragment ions and resolution of two pairs of isobars. Fragmentation mechanisms and ion structures have been proposed.

  9. Development of a dedicated isotope mass spectrometer for the noninvasive diagnostics of humans infected with Helicobacter Pylori

    Science.gov (United States)

    Blashenkov, N. M.; Sheshenya, E. S.; Solov'ev, S. M.; Gall', L. N.; Sachenko, V. M.; Zarutskii, I. V.; Gall', N. R.

    2013-06-01

    A dedicated isotope mass spectrometer for the noninvasive diagnostics of humans infected with Helicobacter Pylori using the isotope respiratory test is developed. A low-aberration mass analyzer is calculated, an input system that makes it possible to eliminate the memory effects is developed, and a small-size ion detector is constructed. The mass spectrometer is created, and the tests are performed. The measurement accuracy of the 13C/12C and 16O/18O isotope ratios are 1.7 and 2.2‰, respectively. Preliminary medical tests show that the spectrometer can be employed for the desired diagnostics.

  10. [Determination of Total Sulfur Dioxide in Chinese Herbal Medicines via Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry].

    Science.gov (United States)

    Wang, Xiao-wei; Liu, Jing-fu; Guan, Hong; Wang, Xiao-yan; Shag, Bing; Zhang, Jing; Liu, Li-ping; Zhang, Ni-na

    2016-02-01

    As an important treatment method, sulfur fumigation plays an essential role in the production and preservation of traditional Chinese herbal medicines. Although there is strict regulation on the use of sulfur dioxide, the abuse of sulfur dioxide still occurred from time to time. And the public faces a high risk of exposure. Because of the poor precision and tedious preparation procedures of traditional recommended titration, the accurate and convenient determination of sulfur dioxide in Chinese herbal medicines is still a critical analytical task for medicines safety and the public health. In this study, an accurate, high-throughput, and convenient method for the absolute determination of SO₂ in Chinese herbal medicines based on triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS/MS) technique is developed. The study compared the quantitative ability for sulfur when the ICP-MS operated under traditional single quadrupole (QMS) mode and novel triple quadrupole (MS/MS) mode with three Reaction/Collision cell condition (no gas, helium, and oxygen). The result indicated that when the concentration of sulfate ranging from 0.5 to 100 mg · L⁻¹, isotopic ³⁴S can be selected as quantitative ion either the ICP-MS operated under the QMS mode or MS/MS mode. The use of helium in the Reaction/Collision cell decreased the single intensity of background ions. Better than QMS mode, the MS/MS mode can effectively reduced background interference. But there are no significant differences about the linear range and limit of detection. However, when the ICP-MS operated under MS/MS mode and oxygen was used as reaction gas in the Reaction/Collision cell, the ICP-MS/MS provided an interference-free performance, the linear range and limit of detection improved significantly. Either ³²S or ³⁴S exhibits an excellent linearity (r > 0.999) over the concentration range of 0.02-100 mg · L⁻¹, with a limit of detection of 5.48 and 9.76 µg · L⁻¹ for

  11. Solid Phase Microextraction and Miniature Time-of-Flight Mass Spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Hiller, j.m.

    1999-01-26

    A miniature mass spectrometer, based on the time-of-flight principle, has been developed for the detection of chemical warfare agent precursor molecules. The instrument, with minor modifications, could fulfill many of the needs for sensing organic molecules in various Defense Programs, including Enhanced Surveillance. The basic footprint of the instrument is about that of a lunch box. The instrument has a mass range to about 300, has parts-per-trillion detection limits, and can return spectra in less than a second. The instrument can also detect permanent gases and is especially sensitive to hydrogen. In volume, the device could be manufactured for under $5000.

  12. Accurate Mass GC/LC-Quadrupole Time of Flight Mass Spectrometry Analysis of Fatty Acids and Triacylglycerols of Spicy Fruits from the Apiaceae Family

    Science.gov (United States)

    Nguyen, Thao; Aparicio, Mario; Saleh, Mahmoud A.

    2016-01-01

    The triacylglycerol (TAG) structure and the regio-stereospecific distribution of fatty acids (FA) of seed oils from most of the Apiaceae family are not well documented. The TAG structure ultimately determines the final physical properties of the oils and the position of FAs in the TAG molecule affects the digestion; absorption and metabolism; and physical and technological properties of TAGs. Fixed oils from the fruits of dill (Anethum graveolens), caraway (Carum carvi), cumin (Cuminum cyminum), coriander (Coriandrum sativum), anise (Pimpinella anisum), carrot (Daucus carota), celery (Apium graveolens), fennel (Foeniculum vulgare), and Khella (Ammi visnaga), all from the Apiaceae family, were extracted at room temperature in chloroform/methanol (2:1 v/v) using percolators. Crude lipids were fractionated by solid phase extraction to separate neutral triacylglycerols (TAGs) from other lipids components. Neutral TAGs were subjected to transesterification process to convert them to their corresponding fatty acids methyl esters (FAMES) using 1% boron trifluoride (BF3) in methanol. FAMES were analyzed by gas chromatography-quadrupole time of flight (GC-QTOF) mass spectrometry. Triglycerides were analyzed using high performance liquid chromatography-quadrupole time of flight (LC-QTOF) mass spectrometry. Petroselinic acid was the major fatty acid in all samples ranging from 57% of the total fatty acids in caraway up to 82% in fennel. All samples contained palmitic (16:0), palmitoleic (C16:1n-9), stearic (C18:0), petroselinic (C18:1n-12), linoleic (C18:2n-6), linolinic (18:3n-3), and arachidic (C20:0) acids. TAG were analyzed using LC-QTOF for accurate mass identification and mass spectrometry/mass spectrometry (MS/MS) techniques for regiospesific elucidation of the identified TAGs. Five major TAGs were detected in all samples but with different relative concentrations in all of the tested samples. Several other TAGs were detected as minor components and were present in

  13. Accurate Mass GC/LC-Quadrupole Time of Flight Mass Spectrometry Analysis of Fatty Acids and Triacylglycerols of Spicy Fruits from the Apiaceae Family.

    Science.gov (United States)

    Nguyen, Thao; Aparicio, Mario; Saleh, Mahmoud A

    2015-12-02

    The triacylglycerol (TAG) structure and the regio-stereospecific distribution of fatty acids (FA) of seed oils from most of the Apiaceae family are not well documented. The TAG structure ultimately determines the final physical properties of the oils and the position of FAs in the TAG molecule affects the digestion; absorption and metabolism; and physical and technological properties of TAGs. Fixed oils from the fruits of dill (Anethum graveolens), caraway (Carum carvi), cumin (Cuminum cyminum), coriander (Coriandrum sativum), anise (Pimpinella anisum), carrot (Daucus carota), celery (Apium graveolens), fennel (Foeniculum vulgare), and Khella (Ammi visnaga), all from the Apiaceae family, were extracted at room temperature in chloroform/methanol (2:1 v/v) using percolators. Crude lipids were fractionated by solid phase extraction to separate neutral triacylglycerols (TAGs) from other lipids components. Neutral TAGs were subjected to transesterification process to convert them to their corresponding fatty acids methyl esters (FAMES) using 1% boron trifluoride (BF₃) in methanol. FAMES were analyzed by gas chromatography-quadrupole time of flight (GC-QTOF) mass spectrometry. Triglycerides were analyzed using high performance liquid chromatography-quadrupole time of flight (LC-QTOF) mass spectrometry. Petroselinic acid was the major fatty acid in all samples ranging from 57% of the total fatty acids in caraway up to 82% in fennel. All samples contained palmitic (16:0), palmitoleic (C16:1n-9), stearic (C18:0), petroselinic (C18:1n-12), linoleic (C18:2n-6), linolinic (18:3n-3), and arachidic (C20:0) acids. TAG were analyzed using LC-QTOF for accurate mass identification and mass spectrometry/mass spectrometry (MS/MS) techniques for regiospesific elucidation of the identified TAGs. Five major TAGs were detected in all samples but with different relative concentrations in all of the tested samples. Several other TAGs were detected as minor components and were present in

  14. Accurate Mass GC/LC-Quadrupole Time of Flight Mass Spectrometry Analysis of Fatty Acids and Triacylglycerols of Spicy Fruits from the Apiaceae Family

    Directory of Open Access Journals (Sweden)

    Thao Nguyen

    2015-12-01

    Full Text Available The triacylglycerol (TAG structure and the regio-stereospecific distribution of fatty acids (FA of seed oils from most of the Apiaceae family are not well documented. The TAG structure ultimately determines the final physical properties of the oils and the position of FAs in the TAG molecule affects the digestion; absorption and metabolism; and physical and technological properties of TAGs. Fixed oils from the fruits of dill (Anethum graveolens, caraway (Carum carvi, cumin (Cuminum cyminum, coriander (Coriandrum sativum, anise (Pimpinella anisum, carrot (Daucus carota, celery (Apium graveolens, fennel (Foeniculum vulgare, and Khella (Ammi visnaga, all from the Apiaceae family, were extracted at room temperature in chloroform/methanol (2:1 v/v using percolators. Crude lipids were fractionated by solid phase extraction to separate neutral triacylglycerols (TAGs from other lipids components. Neutral TAGs were subjected to transesterification process to convert them to their corresponding fatty acids methyl esters (FAMES using 1% boron trifluoride (BF3 in methanol. FAMES were analyzed by gas chromatography-quadrupole time of flight (GC-QTOF mass spectrometry. Triglycerides were analyzed using high performance liquid chromatography-quadrupole time of flight (LC-QTOF mass spectrometry. Petroselinic acid was the major fatty acid in all samples ranging from 57% of the total fatty acids in caraway up to 82% in fennel. All samples contained palmitic (16:0, palmitoleic (C16:1n-9, stearic (C18:0, petroselinic (C18:1n-12, linoleic (C18:2n-6, linolinic (18:3n-3, and arachidic (C20:0 acids. TAG were analyzed using LC-QTOF for accurate mass identification and mass spectrometry/mass spectrometry (MS/MS techniques for regiospesific elucidation of the identified TAGs. Five major TAGs were detected in all samples but with different relative concentrations in all of the tested samples. Several other TAGs were detected as minor components and were present in some

  15. Mass spectra of benzaldehyde using time resolved ion trapping mass spectrometer. Jikan bunkai ion trapping shitsuryo bunsekikei ni yoru benzaldehyde no mass spector

    Energy Technology Data Exchange (ETDEWEB)

    Ishigane, M.; Isa, K. (Fukui Univ., Fukui (Japan). Faculty of Education); Nishioka, K. (Fukui Univ., Fukui (Japan). Faculty of Engineering)

    1991-12-28

    An ion trapping mass spectrometer for time resolved analysis has been set up. The time resolved analysis function of this system is excellent and the ion detecting sensitivity is also high. Benzaldehyde is used as the specimen for the measurement of the A group of the mass spectra (m/z 105 106 and 107) by this system and similar mass spectra are obtained at delay time zero to those reported by now. Big changes are observed in the spectra when the delay times are varied. It is found that mass spectra which are different from those reported already are obtained when the mass spectrometer is pulse operated. In other words it can be said that the time dependence of the data on ion decomposition ( fragmentation) and ion/molecule reactions can be obtained in the state where solvent has no influence if this new system is adopted. 6 refs. 12 figs.

  16. Rapid and accurate U-Th dating of ancient carbonates using inductively coupled plasma-quadrupole mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Douville, Eric; Salle, Eline; Frank, Norbert; Pons-Branchu, Edwige; Ayrault, Sophie [Laboratoire des Sciences du Climat et de l' Environnement, LSCE/IPSL, UMR 8212 CNRS-CEA-UVSQ, Domaine du CNRS, F-91198 Gif/Yvette (France); Eisele, Markus [MARUM, University of Bremen, Leobener Str., 28359 Bremen (DE)

    2010-07-01

    Here, the potential for rapid and accurate U-Th dating technique of marine aragonite skeletons (deep-sea corals, Lophelia pertusa) and secondary calcite deposits (speleothems and stalagmites) has been explored using inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS). The analytical procedure includes a largely simplified chemical separation technique for uranium (U) and thorium (Th) using UTEVA resin. The developed technique permits simultaneous quantification of uranium [{sup 238}U] and thorium [{sup 232}Th] concentrations and their respective isotopic composition, required for U-series disequilibrium dating. Up to 50 U-Th dates per day can be achieved through ICP-QMS with {delta}{sup 234}U and {delta}{sup 230}Th reproducibility (2 {sigma}) of 3-4 parts per thousand and 1%, respectively. The high sensitivity ({>=}3.0 x 10{sup 5} cps/ppb) together with low background ({<=}0.5 cps) on each mass between 228 and 236 amu allowed U-Th dating of ancient deep-water corals (15-260 kyr) and stalagmites (30-85 kyr) at precision levels of less than 2%. Consequently, the combination of simplified chemistry using UTEVA with state-of-the-art ICP-QMS isotopic measurements that do not require a U-Th separation step now provides an extremely rapid and low-cost U-series dating technology. The level of precision is most convenient for numerous geochronological applications, such as the determination of climatic influences on ecosystem development and carbonate precipitation. As a first-example application we present ICP-QMS U-Th dates of North Atlantic deep-water coral fragments retrieved in the southeastern Porcupine Seabight (MD01-2463G. Mound Therese), indicating a purely interglacial growth of deep-water corals on so-called carbonate mounds over several climate cycles. (authors)

  17. Determination of Dicyandiamide in Powdered Milk Using Direct Analysis in Real Time Quadrupole Time-of-Flight Tandem Mass Spectrometry

    Science.gov (United States)

    Zhang, Liya; Yong, Wei; Liu, Jiahui; Wang, Sai; Chen, Qilong; Guo, Tianyang; Zhang, Jichuan; Tan, Tianwei; Su, Haijia; Dong, Yiyang

    2015-08-01

    The direct analysis in real time (DART) ionization source coupled with quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS) system has the capability to desorb analytes directly from samples without sample cleanup or chromatographic separation. In this work, a method based on DART/Q-TOF MS/MS has been developed for rapid identification of dicyandiamide (DCD) present in powdered milk. Simple sample extraction procedure employing acetonitrile-water (80:20, v/v) mixture was followed by direct, high-throughput determination of sample extracts spread on a steel mesh of the transmission module by mass spectrometry under ambient conditions. The method has been evaluated for both qualitative and quantitative analysis of DCD in powdered milk. Variables including experimental apparatus, DART gas heater temperature, sample presentation speed, and vacuum pressure were investigated. The quantitative method was validated with respect to linearity, sensitivity, repeatability, precision, and accuracy by using external standards. After optimization of these parameters, a limit of detection (LOD) of 100 μg kg-1 was obtained for DCD with a linear working range from 100 to 10000 μg kg-1 and a satisfactory correlation coefficient (R2) of 0.9997. Good recovery (80.08%-106.47%) and repeatability (RSD = 3.0%-5.4%) were achieved for DCD. The DART/Q-TOF MS/MS-based method provides a rapid, efficient, and powerful scheme to analyze DCD in powdered milk with limited sample preparation, thus reducing time and complexity of quality control.

  18. Fragmentation pathways of synthetic and naturally occurring coumarin derivatives by ion trap and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Liang, Xianrui; Han, Xiaomei

    2015-09-15

    Synthetic and natural coumarin derivatives possess a wide range of biological activities. Fragmentation pathway studies are important in identifying both naturally occurring coumarins and synthetic coumarins with novel structures and properties. The fragmentation pathways of eleven coumarin derivatives are investigated by electrospray ionization (ESI) ion-trap mass spectrometry (ESI-ITMS(n) ) and ESI quadrupole time-of-flight mass spectrometry (QTOFMS) in positive mode. Compounds 1-9 in this study were newly synthesized in our laboratory. Compounds 10 and 11 were isolated from the root of Zanthoxylum armatum. The major fragmentation pathways for 11 coumarin derivatives are greatly affected by the heterocyclic ring structures and the side-chain substituents. Typical losses of small neutral molecules, such as CH3 CH2 OH, CH2 =CH2 , CO, and H2 O, are observed for compounds 1-5. Compounds 6-9 share similar fragmentation pathways through losses of CO, aromatic rings, and the coumarin skeleton. The main product ions at m/z 205, 219, and 220 observed for compounds 10 and 11 are produced by the loss of C5 H12 O2 , C4 H10 O2 , and the C4 H9 O2 radical, respectively. The fragmentation pathways of 11 coumarin derivatives are elucidated based on ITMS(n) and QTOFMS spectral data. Differences in the structures of the heterocyclic rings and side-chain substituents strongly affect the fragmentation pathways of the coumarins. The present results will facilitate further research into the fragmentation pathways and structural characterization of these classes of compounds with diverse structures. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

  19. In Situ Geochemical Analysis and Age Dating of Rocks Using Laser Ablation-Miniature Mass Spectrometer

    Science.gov (United States)

    Sinha, Mahadeva P.; Hecht, Michael H.; Hurowitz, Joel A.

    2012-01-01

    A miniaturized instrument for performing chemical and isotopic analysis of rocks has been developed. The rock sample is ablated by a laser and the neutral species produced are analyzed using the JPL-invented miniature mass spectrometer. The direct sampling of neutral ablated material and the simultaneous measurement of all the elemental and isotopic species are the novelties of this method. In this laser ablation-miniature mass spectrometer (LA-MMS) method, the ablated neutral atoms are led into the electron impact ionization source of the MMS, where they are ionized by a 70-eV electron beam. This results in a secondary ion pulse typically 10-100 microsecond wide, compared to the original 5-10-nanosecond laser pulse duration. Ions of different masses are then spatially dispersed along the focal plane of the magnetic sector of the miniature mass spectrometer and measured in parallel by a modified CCD (charge-coupled device) array detector capable of detecting ions directly. Compared to conventional scanning techniques, simultaneous measurement of the ion pulse along the focal plane effectively offers a 100% duty cycle over a wide mass range. LAMMS offers a more quantitative assessment of elemental composition than techniques that detect laser-ionized species produced directly in the ablation process because the latter can be strongly influenced by matrix effects that vary with the structure and geometry of the surface, the laser beam, and the ionization energies of the elements. The measurement of high-precision isotopic ratios and elemental composition of different rock minerals by LAMMS method has been demonstrated. The LA-MMS can be applied for the absolute age determination of rocks. There is no such instrument available presently in a miniaturized version that can be used for NASA space missions. Work is in progress in the laboratory for geochronology of rocks using LA-MMS that is based on K-Ar radiogenic dating technique.

  20. Neutral Mass Spectrometer (NMS) for the Lunar Atmosphere and Dust Environment Explorer (LADEE) Mission

    Science.gov (United States)

    Collier, Michael R.; Mahaffy, Paul R.; Benna, Mehdi; King, Todd T.; Hodges, Richard

    2011-01-01

    The Lunar Atmosphere and Dust Environment Explorer (LADEE) mission currently scheduled for launch in early 2013 aboard a Minotaur V will orbit the moon at a nominal periselene of 50 km to characterized the lunar atmosphere and dust environment. The science instrument payload includes a neutral mass spectrometer as well as an ultraviolet spectrometer and a dust detector. Although to date only He, Ar-40, K, Na and Rn-222 have been firmly identified in the lunar exosphere and arise from the solar wind (He), the lunar regolith (K and Na) and the lunar interior (Ar-40, Rn-222), upper limits have been set for a large number of other species, LADEE Neutral Mass Spectrometer (NMS) observations will determine the abundance of several species and substantially lower the present upper limits for many others. Additionally, LADEE NMS will observe the spatial distribution and temporal variability of species which condense at nighttime and show peak concentrations at the dawn terminator (e,g, Ar-40), possible episodic release from the lunar interior, and the results of sputtering or desorption processes from the regolith. In this presentation, we describe the LADEE NMS hardware and the anticipated science results.

  1. Hybrid Quadrupole-Orbitrap mass spectrometry for quantitative measurement of quorum sensing inhibition.

    Science.gov (United States)

    Todd, Daniel A; Zich, David B; Ettefagh, Keivan A; Kavanaugh, Jeffrey S; Horswill, Alexander R; Cech, Nadja B

    2016-08-01

    Drug resistant bacterial infections cause significant morbidity and mortality worldwide, and new strategies are needed for the treatment of these infections. The anti-virulence approach, which targets non-essential virulence factors in bacteria, has been proposed as one way to combat the problem of antibiotic resistance. Virulence in methicillin-resistant Staphylococcus aureus (MRSA) and many other Gram-positive bacterial pathogens is controlled by the quorum sensing system. Thus, there is excellent therapeutic potential for compounds that target this system. With this project, we have developed and validated a novel approach for measuring quorum sensing inhibition in vitro. Ultraperformance liquid chromatography coupled to mass spectrometry (UPLC-MS) was employed to directly measure one of the important outputs of the quorum sensing system in MRSA, auto-inducing peptide I (AIP I) in bacterial cultures. The method for AIP detection was validated and demonstrated limits of detection and quantification of range of 0.0035μM and 0.10μM, respectively. It was shown that the known quorum sensing inhibitor ambuic acid inhibited AIP I production by a clinically relevant strain of MRSA, with an IC50 value of 2.6±0.2μM. The new method performed similarly to previously published methods using GFP reporter assays, but has the advantage of being applicable without the need for engineering of a reporter strain. Additionally, the mass spectrometry-based method could be applicable in situations where interference by the inhibitor prevents the application of fluorescence-based methods.

  2. Liquid chromatography-quadrupole-time-of-flight mass spectrometry screening procedure for urine samples in forensic casework compared to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fels, Helena; Dame, Torsten; Sachs, Hans; Musshoff, Frank

    2016-07-04

    This work represents the development, validation, and application of a liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) screening method for the detection of pharmaceutical substances and illicit drugs (acidic, basic, and neutral organic drugs) in urine samples. Time-of-flight mass spectrometry was performed using an LC-Triple TOF 5600 system with electrospray ionization operated in both positive and negative mode, respectively. The limits of detection (LODs), determined for 34 substances, were 70%). These four parameters served as identification criteria and are discussed according to their role in identifying compounds even without reference substances. In routine casework, two in-house XIC (extracted ion chromatogram) lists, consisting of 456 protonated and 26 deprotonated compounds were used and retention times for 365 compounds were available. Compared to the results found with the established gas chromatography-mass spectrometry (GC-MS) procedure, the findings with the LC-QTOF-MS screening method showed a good comparability. Results that were not detected by LC-QTOF-MS because of a missing entry in the targeted XIC list could retrospectively be confirmed by simply entering the elemental formula of the relevant substance into the software and reprocessing the sample. LC-QTOF-MS offers an attractive technique for the fast and specific identification of illicit drugs and toxic compounds in urine samples. Copyright © 2016 John Wiley & Sons, Ltd.

  3. Virtual Models of Mass Spectrometers as Teaching Tools for Graduate Students.

    Directory of Open Access Journals (Sweden)

    L. Gomes da Silva

    2010-05-01

    Full Text Available Universidade Federal do Rio de Janeiro – UFRJ – Campus Macaé- RJMass spectrometry is an analytical powerful technique for identifying unknowns, quantitating knows and discovering chemicals properties and molecular structures. The mass spectrometry concept is very simple: The sample becomes an ion through an ionization method. Ions are selected by mass to charge ratio (m/z based upon the motion in a magnetic field and each one is register under a spectrum. To access the basic of these techniques by using appropriate literature, videos, virtual models and simulations for this machinesbehavior is today´s exclusiveness for researchers through manufacturer handbooks. This reality becomes the science popularization and knowledge diffusion about proteomic analysis something plenty arduous for the portion or part of graduate students. The work objectives were making a multimediaschool-book showing biochemical techniques for proteomic analysis using mass spectrometry. The material was make with specific software for building 3D models and animation of different ionizations methods: Electron Ionization (EI, Electro spray Ionization (ESI, Atmospheric Pressure Chemical Ionization(APCI, Matrix Assisted Laser Desorption/Ionization (MALD and mass analyzers: Time of Flight(TOF, Quadrupole and Ion Trap.

  4. 233U mass yield measurements around and within the symmetry region with the ILL Lohengrin spectrometer

    Directory of Open Access Journals (Sweden)

    Chebboubi A.

    2016-01-01

    Full Text Available The study of fission yields has a major impact on the characterization and understanding of the fission process and is mandatory for reactor applications. The LPSC in collaboration with ILL and CEA has developed a measurement program on fission fragment distributions at the Lohengrin spectrometer of the ILL, with a special focus on the masses constituting the heavy peak. We will present in this paper our measurement of the very low fission yields in the symmetry mass region and the heavy mass wing of the distribution for 233U thermal neutron induced fission. The difficulty due to the strong contamination by other masses with much higher yields will be addressed in the form of a new analysis method featuring the required contaminant correction. The apparition of structures in the kinetic energy distributions and possible interpretations will be discussed, such as a possible evidence of fission modes.

  5. 233U mass yield measurements around and within the symmetry region with the ILL Lohengrin spectrometer

    Science.gov (United States)

    Chebboubi, A.; Kessedjian, G.; Sage, C.; Bernard, D.; Blanc, A.; Faust, H.; Köster, U.; Litaize, O.; Mutti, P.; Serot, O.

    2016-03-01

    The study of fission yields has a major impact on the characterization and understanding of the fission process and is mandatory for reactor applications. The LPSC in collaboration with ILL and CEA has developed a measurement program on fission fragment distributions at the Lohengrin spectrometer of the ILL, with a special focus on the masses constituting the heavy peak. We will present in this paper our measurement of the very low fission yields in the symmetry mass region and the heavy mass wing of the distribution for 233U thermal neutron induced fission. The difficulty due to the strong contamination by other masses with much higher yields will be addressed in the form of a new analysis method featuring the required contaminant correction. The apparition of structures in the kinetic energy distributions and possible interpretations will be discussed, such as a possible evidence of fission modes.

  6. Rapid Detection of Gas Hazards and Leaks with an Atmospheric Sampling, High Resolution, Mass Spectrometer with Low Pumping Requirements Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Miniaturization of mass spectrometers is restricted almost exclusively by the ability of small vacuum pumps to remove gas loads during operation of the instrument....

  7. Influence of the coupling between an atmospheric pressure ion mobility spectrometer and the low pressure ion inlet of a mass spectrometer on the mobility measurement

    Directory of Open Access Journals (Sweden)

    Gunzer Frank

    2016-01-01

    Full Text Available Ion mobility spectrometers (IMS are versatile gas analyzers. Due to their small size and robustness, combined with a very high sensitivity, they are often used in gas sensing applications such as environmental monitoring. In order to improve the selectivity, they are typically combined with a mass spectrometer (MS. Since IMS works at atmospheric pressure, and MS works at vacuum, a special interface reducing the pressure over normally two stages has to be used. In this paper the influence of this coupling of different pressure areas on the IMS signal will be analyzed with help of finite elements method simulations.

  8. Design of New Electrode Interface to Improve Transport of Atmospheric Pressure Ions into a Mass Spectrometer

    Directory of Open Access Journals (Sweden)

    Francis Beaudry

    2009-01-01

    Full Text Available An intermediate electrode was developed to improve the transfer of ions in atmospheric pressure from a first location, the ion source, to a second location, the mass spectrometer. The new apparatus increase the efficiency of mass analysis of molecular constituents of liquids, including trace analysis of chemical entities, in which an electrospray (ES or IonSpray™ (IS technique is used to produce electrically charged droplets which divide and evaporate to form gaseous ions of the molecular constituents. The gas phase ions are transported to the mass spectrometer by an electric field generated by a new electrode design that separates the two fundamental functions of an electrospray or an IonSpray™, which are the nebulization of charged droplets and the transport of ions into the mass analyzer. The results suggest that the new apparatus provide a gain in signal intensity up to 10 compared with the commercial product. A significant improvement in ion transport results in higher precision and accuracy and/or reduction of the amount of material needed for analysis.

  9. Rapid identification of erythrocyte phospholipids in Sprague-Dawley rats by ultra high performance liquid chromatography with electrospray ionization quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Pi, Juanjuan; Wu, Xia; Yang, Shitian; Zeng, Pingyan; Feng, Yifan

    2015-03-01

    A rapid, sensitive, and reliable approach for analyzing five kinds of erythrocyte phospholipids in Sprague-Dawley rats was provided by ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry with MassLynx(TM) MassFragment. Improving conventional high performance liquid chromatography techniques, ultra high performance liquid chromatography integrated with quadrupole time-of-flight tandem mass spectrometry offers high sensitivity and increased analytical speed by using columns packed with sub-2 μm particles (1.7 μm), which allows a faster separation to be achieved. Through this method, 83 phospholipids were tentatively characterized based on their mass spectra and tandem mass spectra, as well as by matching the in-house formula database within a mass error of 5 ppm, including 40 phosphatidylcholines, 24 phosphatidyl ethanolamines, three phosphatidylinositols, six phosphatidylserines, and ten sphingomyelins. Our present results proved that the established method could be used to qualitatively analyze complex erythrocyte phospholipids in Sprague-Dawley rats and provide a useful data base for pharmacology and phospholipidomics to seek potential biomarkers of disease prediction.

  10. Gas chromatography interfaced with atmospheric pressure ionization-quadrupole time-of-flight-mass spectrometry by low-temperature plasma ionization

    DEFF Research Database (Denmark)

    Norgaard, Asger W.; Kofoed-Sorensen, Vivi; Svensmark, Bo

    2013-01-01

    A low temperature plasma (LTP) ionization interface between a gas chromatograph (GC) and an atmospheric pressure inlet mass spectrometer, was constructed. This enabled time-of-flight mass spectrometric detection of GC-eluting compounds. The performance of the setup was evaluated by injection...

  11. Identification of in vitro metabolites of ethylphenidate by liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Negreira, Noelia; Erratico, Claudio; van Nuijs, Alexander L N; Covaci, Adrian

    2016-01-05

    Ethylphenidate is a new potent synthetic psychoactive drug, structurally related to methylphenidate. Using human liver microsomes and cytosol, we have investigated for the first time the Phase-I and Phase-II in vitro metabolism of ethylphenidate. The structure of the metabolites was elucidated by hybrid quadrupole time-of-flight mass spectrometry. Overall, seven Phase-I, but no Phase-II metabolites were detected. Ethylphenidate underwent hydroxylation forming two primary mono-hydroxylated metabolites and, subsequently, dehydration and ring opening with an additional hydroxylation, forming secondary metabolites. The involvement of different human cytochrome P450 (CYP) enzymes in the formation of ethylphenidate metabolites was investigated using a panel of human recombinant CYPs (rCYPs). rCYP2C19 was the most active recombinant enzyme involved in the formation of all seven ethylphenidate metabolites detected, although other rCYPs (rCYP1A2, rCYP2B6, rCYPC9, rCYP2D6, and rCYP3A4, but not rCYP2E1) played a role in the metabolism of ethylphenidate. All metabolites identified in the present study can be considered as potential specific biomarkers of ethylphenidate in toxicological studies. Additionally, ritalinic acid and methylphenidate were formed by non-enzymatic hydrolysis and trans-esterification, and, therefore, they cannot be considered as (oxidative) metabolites of ethylphenidate. The presence of methylphenidate and ritalinic acid cannot be exclusively associated to the use of ethylphenidate, since methylphenidate is a drug itself and ritanilic acid can be formed from both ethylphenidate and methylphenidate.

  12. [Simultaneous determination of ethyl carbamate and chloropropanols in flavorings by gas chromatography-triple quadrupole tandem mass spectrometry].

    Science.gov (United States)

    Xu, Xiaomin; He, Huali; Ruan, Yudi; Huang, Baifen; Zhang, Jingshun; Cai, Zengxuan; Ren, Yiping

    2013-11-01

    A simultaneous determination method for ethyl carbamate (EC) and chloropropanols (3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD)) in flavorings was developed by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). After spiked with internal standard, the sample was extracted by matrix solid-phase dispersion extraction technique with an Extrelut NT column. Hexane was used to wash the fat soluble matrix interferences and then an ethyl acetate-ethyl ether (20: 80, v/v) mixture was added to elute the analytes. The concentrated extract was detected by GC-MS/MS in multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 2, 5 and 5 microg/kg for EC, 3-MCPD and 2-MCPD, respectively. The linear ranges were 5 - 1 000 microg/kg (r = 0.9997), 10-1000 microg/kg (r = 0.999 1) and 10-1000 microg/kg (r = 0.999 5) for EC, 3-MCPD and 2-MCPD, respectively. In soy sauce, yellow rice wine, salami sauce and flavoring of instant noodle matrices, the recoveries (RSDs, n = 7) in MRM mode at the levels of 20, 100 and 400 microg/kg were 87.7%-104% (4.3%-10.7%), 90.1%-109% (2.6%-10.2%), and 90.9%-103% (3.0%-9.5%), respectively. EC, 3-MCPD and 2-MCPD were found in some real samples of the soy sauce, wine and flavoring of instant noodle. EC or 3-MCPD was found in some of the salami samples. The method is accurate, fast and suitable for the simultaneous determination of EC, 3-MCPD and 2-MCPD in flavorings.

  13. Investigations in the possibility of early detection of colorectal cancer by gas chromatography/triple-quadrupole mass spectrometry.

    Science.gov (United States)

    Nishiumi, Shin; Kobayashi, Takashi; Kawana, Shuichi; Unno, Yumi; Sakai, Takero; Okamoto, Koji; Yamada, Yasuhide; Sudo, Kazuki; Yamaji, Taiki; Saito, Yutaka; Kanemitsu, Yukihide; Okita, Natsuko Tsuda; Saito, Hiroshi; Tsugane, Shoichiro; Azuma, Takeshi; Ojima, Noriyuki; Yoshida, Masaru

    2017-03-07

    In developed countries, the number of patients with colorectal cancer has been increasing, and colorectal cancer is one of the most common causes of cancer death. To improve the quality of life of colorectal cancer patients, it is necessary to establish novel screening methods that would allow early detection of colorectal cancer. We performed metabolome analysis of a plasma sample set from 282 stage 0/I/II colorectal cancer patients and 291 healthy volunteers using gas chromatography/triple-quadrupole mass spectrometry in an attempt to identify metabolite biomarkers of stage 0/I/II colorectal cancer. The colorectal cancer patients included patients with stage 0 (N=79), I (N=80), and II (N=123) in whom invasion and metastasis were absent. Our analytical system detected 64 metabolites in the plasma samples, and the levels of 29 metabolites differed significantly (Bonferroni-corrected p=0.000781) between the patients and healthy volunteers. Based on these results, a multiple logistic regression analysis of various metabolite biomarkers was carried out, and a stage 0/I/II colorectal cancer prediction model was established. The area under the curve, sensitivity, and specificity values of this model for detecting stage 0/I/II colorectal cancer were 0.996, 99.3%, and 93.8%, respectively. The model's sensitivity and specificity values for each disease stage were >90%, and surprisingly, its sensitivity for stage 0, specificity for stage 0, and sensitivity for stage II disease were all 100%. Our predictive model can aid early detection of colorectal cancer and has potential as a novel screening test for cases of colorectal cancer that do not involve lymph node or distant metastasis.

  14. Determination of albendazole and metabolites in silkworm Bombyx mori hemolymph by ultrafast liquid chromatography tandem triple quadrupole mass spectrometry.

    Science.gov (United States)

    Li, Li; Xing, Dong-Xu; Li, Qing-Rong; Xiao, Yang; Ye, Ming-Qiang; Yang, Qiong

    2014-01-01

    Albendazole is a broad-spectrum parasiticide with high effectiveness and low host toxicity. No method is currently available for measuring albendazole and its metabolites in silkworm hemolymph. This study describes a rapid, selective, sensitive, synchronous and reliable detection method for albendazole and its metabolites in silkworm hemolymph using ultrafast liquid chromatography tandem triple quadrupole mass spectrometry (UFLC-MS/MS). The method is liquid-liquid extraction followed by UFLC separation and quantification in an MS/MS system with positive electrospray ionization in multiple reaction monitoring mode. Precursor-to-product ion transitions were monitored at 266.100 to 234.100 for albendazole (ABZ), 282.200 to 208.100 for albendazole sulfoxide (ABZSO), 298.200 to 159.100 for albendazole sulfone (ABZSO2) and 240.200 to 133.100 for albendazole amino sulfone (ABZSO2-NH2). Calibration curves had good linearities with R2 of 0.9905-0.9972. Limits of quantitation (LOQs) were 1.32 ng/mL for ABZ, 16.67 ng/mL for ABZSO, 0.76 ng/mL for ABZSO2 and 5.94 ng/mL for ABZSO2-NH2. Recoveries were 93.12%-103.83% for ABZ, 66.51%-108.51% for ABZSO, 96.85%-105.6% for ABZSO2 and 96.46%-106.14% for ABZSO2-NH2, (RSDs albendazole and its metabolites in silkworm hemolymph in a pharmacokinetic study. The results of single-dose treatment suggested that the concentrations of ABZ, ABZSO and ABZSO2 increased and then fell, while ABZSO2-NH2 level was low without obvious change. Different trends were observed for multi-dose treatment, with concentrations of ABZSO and ABZSO2 rising over time.

  15. Determination of pesticide residues in animal origin baby foods by gas chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Amendola, Graziella; Pelosi, Patrizia; Attard Barbini, Danilo

    2015-01-01

    A simple, fast and multiresidue method for the determination of pesticide residues in baby foods of animal origin has been developed in order to check the compliance with the Maximum Residue Levels (MRLs) set at a general value of 0.01 mg/kg by Commission Directive 2006/125/EC for infant foods. The main classes of organochlorine, organophosphorus and pyrethroid compounds have been considered, which are mainly fat soluble pesticides. The analytical procedure consists in the extraction of baby food samples by acetonitrile (ACN) followed by a clean up using C18 solid-phase extraction column eluted with ACN. The compounds were determined by gas chromatography-triple quadrupole mass spectrometry equipped with a Programmed Temperature Vaporizer (PTV) injection and a backflush system. In order to compensate for matrix effects PTV and matrix matched standard calibrations have been used. The method has been fully validated for 57 pesticides according to the Document SANCO/12571/2013. Accuracy and precision (repeatability) have been studied by recoveries at two spiking levels, the Limit of Quantitation (LOQ) (0.003-0.008 mg/kg) and 10 time greater (0.03-0.08 mg/kg), and the results were in the acceptable range of 70-120% with Relative Standards Deviations (RSD) ≤20%. Selectivity, linearity, LOQ and uncertainty of measurement were also determined for all the compounds. The method has been also applied for the analysis of 18 baby food animal origin samples, bought form the local market in Rome (Italy), and no pesticide in the scope of the method has been found above the MRL or the LOQ.

  16. [Determination of 16 phthalate acid ester residues in health wine by gas chromatography-triple quadrupole mass spectrometry].

    Science.gov (United States)

    Lu, Li; Gong, Xu; Feng, Youlong

    2014-11-01

    A method for the analysis of sixteen phthalate acid ester (PAE) residues in health wine was developed using gas chromatography-triple quadrupole mass spectrometry (GC-QQQ- MS). The health wine samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The samples were detected by GC-QQQ-MS with electron impact source (EI) in selected ion monitoring (SIM) mode after extraction. The separation was performed on an HP-5MS capillary column (30 m x 0.25 mm x 0.25 μm) with temperature programming. The retention time and the fragment ion abundance ratio were used to judge the qualitative results, and the quantitation was performed with standard curve method of the characteristic ion chrom- atographic peak area-concentration. Eighty-one batches of health wine samples were detected using the method. The results showed that the method had good linear relationships with correlation coefficients (r2) not less than 0.995 9. The recoveries of fifteen PAEs ranged from 88.6% to 107. 3% except dimethyl phthalate (DMP) which was 52.3%-58.7% in all the three spiked levels with the relative standard deviations of 0.1%-6.8% (RSD, n = 6). The limits of detection were between 0.002 mg/L to 0.061 mg/L. The limits of quantification were between 0.005 mg/L and 0.202 mg/L. The method is accurate, sensitive, proprietary and suitable for the simultaneous determination of the sixteen phthalate acid esters in health wine.

  17. Formation of solvated ions in the atmospheric interface of an electrospray ionization triple-quadrupole mass spectrometer.

    Science.gov (United States)

    Schlosser, Gitta; Takáts, Zoltán; Vékey, Károly

    2003-12-01

    A simple method capable of generating and investigating various solvent clusters and solvated ions was developed. The technique opens a door to studying these complexes on commercially available instruments. Formation of the desired solvated ion in the gas phase was achieved by introducing the appropriate volatile solvent vapour into the curtain gas stream. Capabilities of the technique are illustrated by generating alkali, alkaline earth and transition metal cations solvated by various volatile compounds such as water, methanol and acetonitrile. Depending on the ligands and on the experimental conditions, clusters of 2-100 molecules may be observed. Isotope labelling suggests that these are formed by a re-solvation process in the curtain gas region.

  18. Rapid and Deep Proteomes by Faster Sequencing on a Benchtop Quadrupole Ultra-High-Field Orbitrap Mass Spectrometer

    DEFF Research Database (Denmark)

    Kelstrup, Christian D; Jersie-Christensen, Rosa R; Batth, Tanveer Singh

    2014-01-01

    per second or up to 600 new peptides sequenced per gradient minute. We identify 4400 proteins from one microgram of HeLa digest using a one hour gradient, which is an approximately 30% improvement compared to previous instrumentation. In addition, we show very deep proteome coverage can be achieved...... in less than 24 hours of analysis time by offline high pH reversed-phase peptide fractionation from which we identify more than 140,000 unique peptide sequences. This is comparable to state-of-the-art multi-day, multi-enzyme efforts. Finally the acquisition methods are evaluated for single...

  19. Identification of isomers and control of ionization and dissociation processes using dual-mass-spectrometer scheme and genetic algorithm optimization

    Institute of Scientific and Technical Information of China (English)

    陈洲; 佟秋男; 张丛丛; 胡湛

    2015-01-01

    Identification of acetone and its two isomers, and the control of their ionization and dissociation processes are per-formed using a dual-mass-spectrometer scheme. The scheme employs two sets of time of flight mass spectrometers to simultaneously acquire the mass spectra of two different molecules under the irradiation of identically shaped femtosecond laser pulses. The optimal laser pulses are found using closed-loop learning method based on a genetic algorithm. Com-pared with the mass spectra of the two isomers that are obtained with the transform limited pulse, those obtained under the irradiation of the optimal laser pulse show large differences and the various reaction pathways of the two molecules are selectively controlled. The experimental results demonstrate that the scheme is quite effective and useful in studies of two molecules having common mass peaks, which makes a traditional single mass spectrometer unfeasible.

  20. Polymer and Additive Mass Spectrometry Literature Review

    Energy Technology Data Exchange (ETDEWEB)

    Shear, Trevor Allan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-06-06

    The use of mass spectrometry in fields related to polymers has increased significantly over the past three decades and will be explored in this literature review. The importance of this technique is highlighted when exploring how polymers degrade, verifying purchased materials, and as internal requirements change. The primary focus will be on four ionization techniques and the triple quadrupole and quadrupole / time-of-flight mass spectrometers. The advantages and limitations of each will also be explored.

  1. Feasibility of using a miniature NIR spectrometer to measure volumic mass during alcoholic fermentation.

    Science.gov (United States)

    Fernández-Novales, Juan; López, María-Isabel; González-Caballero, Virginia; Ramírez, Pilar; Sánchez, María-Teresa

    2011-06-01

    Volumic mass-a key component of must quality control tests during alcoholic fermentation-is of great interest to the winemaking industry. Transmitance near-infrared (NIR) spectra of 124 must samples over the range of 200-1,100-nm were obtained using a miniature spectrometer. The performance of this instrument to predict volumic mass was evaluated using partial least squares (PLS) regression and multiple linear regression (MLR). The validation statistics coefficient of determination (r(2)) and the standard error of prediction (SEP) were r(2) = 0.98, n = 31 and r(2) = 0.96, n = 31, and SEP = 5.85 and 7.49 g/dm(3) for PLS and MLR equations developed to fit reference data for volumic mass and spectral data. Comparison of results from MLR and PLS demonstrates that a MLR model with six significant wavelengths (P alcoholic fermentation, and that a low-cost NIR instrument can be used for this purpose.

  2. An indigenous cluster beam apparatus with a reflectron time-of-flight mass spectrometer

    Indian Academy of Sciences (India)

    G Raina; G U Kulkarni; R T Yadav; V S Ramamurthy; C N R Rao

    2000-04-01

    The design and fabrication of a Smalley-type cluster source in combination with a reflectron based time-of-flight (TOF) mass spectrometer are reported. The generation of clusters is based on supersonic jet expansion of the sampling plume. Sample cells for both liquid and solid targets developed for this purpose are described. Two pulsed Nd-YAG lasers are used in tandem, one (532 nm) for target vapourization and the other (355 nm) for cluster ionization. Methanol clusters of nuclearity up to 14 (mass 500 amu) were produced from liquid methanol as the test sample. The clusters were detected with a mass resolution of ~ 2500 in the R-TOF geometry. Carbon clusters up to a nuclearity of 28 were obtained using a polyimide target. The utility of the instrument is demonstrated by carrying out experiments to generate mixed clusters from alcohol mixtures.

  3. Advanced Ion Mass Spectrometer for Giant Planet Ionosphere, Magnetospheres and Moons

    Science.gov (United States)

    Sittler, Edward; Cooper, John; Paschalidis, Nick; Jones, Sarah; Brinkerhoff, William; Paterson, William; Ali, Ashraf; Coplan, Michael; Chornay, Dennis; Sturner, Steve; Benna, Mehdi; Bateman, Fred; Fontaine, Dominique; Verdeil, Christophe; Andre, Nicolas; Blanc, Michel; Wurz, Peter

    2017-01-01

    We present our Advanced Ion Mass Spectrometer (AIMS) for outer planet missions which has been under development from various NASA sources (NASA Living with a Star Instrument Development (LWSID), NASA Astrobiology Instrument Development (ASTID), NASA Goddard Internal Research and Development (IRAD)s) to measure elemental, isotopic, and simple molecular composition abundances of 1 V to 25 kV hot ions with wide field-of-view (FOV) in the 1 - 60 amu mass range at mass resolution M/ ΔM radiation background from the inner magnetospheres of Jupiter and Saturn to the outer magnetospheric boundary regions and the upstream solar wind. This instrument will work for both spinning spacecraft and 3-axis stabilized spacecraft. AIMS will measure the ion velocity distribution functions (VDF) for the individual ion species from which velocity moments will give their ion density, flow velocity and temperature.

  4. Normal phase liquid chromatography coupled to quadrupole time of flight atmospheric pressure chemical ionization mass spectrometry for separation, detection and mass spectrometric profiling of neutral sphingolipids and cholesterol.

    Science.gov (United States)

    Farwanah, Hany; Wirtz, Jennifer; Kolter, Thomas; Raith, Klaus; Neubert, Reinhard H H; Sandhoff, Konrad

    2009-10-01

    Many lipidomic approaches focus on investigating aspects of sphingolipid metabolism. Special emphasis is put on neutral sphingolipids and cholesterol and their interaction. Such an interest is attributed to the fact that those lipids are altered in a series of serious disorders including various sphingolipidoses. High performance thin-layer chromatography (HPTLC) has become a widely used technique for lipid analysis. However, mass spectrometric profiling is irreplaceable for gaining an overview about the various molecular species within a lipid class. In this work we have developed a sensitive method based on a gradient normal phase high performance liquid chromatography (HPLC) coupled to quadrupole time of flight (QTOF) atmospheric pressure chemical ionization mass spectrometry (APCI-MS) in positive mode, which for the first time enables separation, on-line detection, and mass spectrometric profiling of multiple neutral sphingolipids including ceramide, glucosylceramide, lactosylceramide, globotriaosylceramide, globotetraosylceramide, sphingomyelin as well as cholesterol within less than 15min. An important advantage of the presented HPLC/APCI-MS approach is that the separation pattern emulates the one obtained by an optimized HPTLC method with a multiple stage development. Thus, the lipid classes previously separated and quantified by HPTLC can be easily screened regarding their mass spectrometric profiles by HPLC/APCI-MS. In addition, the selected ionization conditions enable in-source fragmentation providing useful structural information. The methods (HPLC/APCI-MS and the optimized HPTLC) were applied for the analysis of the mentioned lipids in human fibroblasts. This approach is aimed basically at investigators who perform studies based on genetic modifications or treatment with pharmacological agents leading to changes in the biochemical pathways of neutral sphingolipids and cholesterol. In addition, it can be of interest for research on disorders related to

  5. Development of electrospray ionization of biomolecules on a magnetic sector mass spectrometer

    CERN Document Server

    Zhang, Y

    2002-01-01

    The initial part of this study involves developments made on an electrospray ionization (ESI) source installed on a large-scale double-focusing reverse-geometry two-sector mass spectrometer. The practical considerations and some basic theory have been given in this thesis for each of the improvements made to the ESI source. The process of partial re-designing the ion optical system showed that the ion beam was affected by both gas dynamics and by the field penetration from the lenses of the ion optical system in the region immediately after second skimmer. More than one order magnitude stronger ion signal intensities at the mass spectrometer final detector and easier ESI source operation conditions and stable ion signals has been achieved. Mass-analyzed ion kinetic energy spectroscopy (MIKES) of different charge-states of relatively small peptides (substance P and bradykinin) for collision-induced dissociation (CID) and the metastable dissociation was carried out successfully. The translational energy losses ...

  6. GoAmazon 2014/15 Thermal Desorption Chemical Ionization Mass Spectrometer (TDCIMS) Field Campaign Report

    Energy Technology Data Exchange (ETDEWEB)

    Smith, JN [Univ. of California, Irvine, CA (United States)

    2016-04-01

    The Thermal Desorption Chemical Ionization Mass Spectrometer (TDCIMS) deployment to the U.S. Department of Energy (DOE)’s Atmospheric Radiation Measurement (ARM) Climate Research Facility T3 site in Manacapuru, Brazil, was motivated by two main scientific objectives of the Green Ocean Amazon (GoAmazon) 2014/15 field campaign. 1) Study the interactions between anthropogenic and biogenic emissions by determining important molecular species in ambient nanoparticles. To address this, TDCIMS data will be combined with coincident measurements such as gas-phase sulfuric acid to determine the contribution of sulfuric acid condensation to nucleation and growth. We can then compare that result to TDCIMS-derived nanoparticle composition to determine the fraction of growth that can be attributed to the uptake of organic compounds. The molecular composition of sampled particles will also be used to attribute specific chemical species and mechanisms to growth, such as the condensation of low-volatility species or the oligomerization of α-dicarbonyl compounds. 2) Determine the source of new ambient nanoparticles in the Amazon. The hypothesis prior to measurements was that potassium salts formed from the evaporation of primary particles emitted by fungal spores can provide a unique and important pathway for new particle production in the Amazon basin. To explore this hypothesis, the TDCIMS recorded the mass spectra of sampled ambient particles using a protonated water cluster Chemical Ionization Mass Spectrometer (CIMS). Laboratory tests performed using potassium salts show that the TDCIMS can detect potassium with high sensitivity with this technique.

  7. In situ analysis of corrosion inhibitors using a portable mass spectrometer with paper spray ionization

    KAUST Repository

    Jjunju, Fred Paul Mark

    2013-01-01

    Paper spray (PS) ambient ionization is implemented using a portable mass spectrometer and applied to the detection of alkyl quaternary ammonium salts in a complex oil matrix. These salts are commonly used as active components in the formulation of corrosion inhibitors. They were identified in oil and confirmed by their fragmentation patterns recorded using tandem mass spectrometry (MS/MS). The cations of alkyl and benzyl-substituted quaternary ammonium salts showed characteristic neutral losses of CnH2n (n carbon number of the longest chain) and C7H8, respectively. Individual quaternary ammonium compounds were detected at low concentrations (<1 ng μL-1) and over a dynamic range of ∼5 pg μL-1 to 500 pg μL-1 (ppb). Direct detection of these compounds in complex oil samples without prior sample preparation or pre-concentration was also demonstrated using a home-built miniature mass spectrometer at levels below 1 ng μL-1.© 2013 The Royal Society of Chemistry.

  8. Feasibility of a Fieldable Mass Spectrometer FY 2015 Year-end Report

    Energy Technology Data Exchange (ETDEWEB)

    Barinaga, Charles J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hager, George J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hoegg, Edward D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Carman, April J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hart, Garret L. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2015-10-01

    Currently, the International Atomic Energy Agency (IAEA) monitors the production of enriched uranium hexafluoride (UF6) at declared facilities by collecting a few grams of product in sample tubes that are then sent to central laboratories for processing and isotope ratio analysis by thermal ionization mass spectrometry. Analysis of results may not be available for some time after collection. In addition, new shipping regulations will make it more difficult to transport this amount of UF6 to a laboratory. The IAEA is interested in an isotope ratio technique for uranium in UF6 that can be moved to and operated at the enrichment facility itself. This report covers the tasks and activities of the Feasibility of a Fieldable Mass Spectrometer Project for FY 2015, which investigates the feasibility of an in-field isotope ratio technique— the forward deployment of a technique to the non-laboratory situation of a protected room with power and heat at the facility of interest. A variety of nontraditional elemental ionization techniques were considered. It was determined that only two of these should be moved forward for testing with the candidate in-field mass spectrometer and with the adsorbed UF6 sample types.

  9. In situ analysis of corrosion inhibitors using a portable mass spectrometer with paper spray ionization.

    Science.gov (United States)

    Jjunju, Fred P M; Li, Anyin; Badu-Tawiah, Abraham; Wei, Pu; Li, Linfan; Ouyang, Zheng; Roqan, Iman S; Cooks, R Graham

    2013-07-01

    Paper spray (PS) ambient ionization is implemented using a portable mass spectrometer and applied to the detection of alkyl quaternary ammonium salts in a complex oil matrix. These salts are commonly used as active components in the formulation of corrosion inhibitors. They were identified in oil and confirmed by their fragmentation patterns recorded using tandem mass spectrometry (MS/MS). The cations of alkyl and benzyl-substituted quaternary ammonium salts showed characteristic neutral losses of CnH2n (n carbon number of the longest chain) and C7H8, respectively. Individual quaternary ammonium compounds were detected at low concentrations (<1 ng μL(-1)) and over a dynamic range of ∼5 pg μL(-1) to 500 pg μL(-1) (ppb). Direct detection of these compounds in complex oil samples without prior sample preparation or pre-concentration was also demonstrated using a home-built miniature mass spectrometer at levels below 1 ng μL(-1).

  10. Matrix-assisted ionization vacuum for high-resolution Fourier transform ion cyclotron resonance mass spectrometers.

    Science.gov (United States)

    Wang, Beixi; Tisdale, Evgenia; Trimpin, Sarah; Wilkins, Charles L

    2014-07-15

    Matrix-assisted ionization vacuum (MAIV) produces charge states similar to electrospray ionization (ESI) from the solid state without requiring high voltage or added heat. MAIV differs from matrix-assisted laser desorption/ionization (MALDI) in that no laser is needed and abundant multiply charged ions are produced from molecules having multiple basic sites such as proteins. Here we introduce simple modifications to the commercial vacuum MALDI and ESI sources of a 9.4 T Fourier transform-ion cyclotron resonance (FT-ICR) mass spectrometer to perform MAIV from both intermediate and atmospheric pressure. The multiply charged ions are shown for the proteins bovine insulin, ubiquitin, and lysozyme using 3-nitrobenzonitrile as matrix. These are the first examples of MAIV operating at pressures as low as 10(-6) mbar in an FT-ICR mass spectrometer source, and the expected mass resolving power of 100000 to 400000 is achieved. Identical protein charge states are observed with and without laser ablation indicating minimal, if any, role of photochemical ionization for the compounds studied.

  11. Delayed extraction time-of-flight mass spectrometer with electron impact for PAH studies

    Science.gov (United States)

    Najeeb, P. K.; Kadhane, U.

    2017-03-01

    A time-of-flight (ToF) mass spectrometer with a pulsed electron beam as well as pulsed extraction of the recoil ions, with variable delay is reported. The effectiveness of this technique is highlighted by studying the statistical decay of mono-cations over microsecond time scales. Various details of the design and operation are discussed in the context of electron impact ionization and fragmentation of naphthalene (C10H8). The temporal behavior of acetylene (C2H2) and diacetylene (C4H2) loss is observed and compared with the associated Arrhenius decay constant, internal energy and plasmon excitation energy.

  12. Accurate mass measurements of short-lived isotopes with the MISTRAL rf spectrometer

    CERN Document Server

    Toader, C F; Borcea, C; Doubre, H; Duma, M; Jacotin, M; Henry, S; Képinski, J F; Lebée, G; Le Scornet, G; Lunney, M D; Monsanglant, C; De Saint-Simon, M; Thibault, C

    1999-01-01

    The MISTRAL experiment has measured its first masses at ISOLDE. Installed in May 1997, this radiofrequency transmission spectrometer is to concentrate on nuclides with particularly short half-lives. MISTRAL received its first stable beam in October and first radioactive beam in November 1997. These first tests, with a plasma ion source, resulted in excellent isobaric separation and reasonable transmission. Further testing and development enabled first data taking in July 1998 on neutron-rich Na isotopes having half-lives as short as 31 ms.

  13. Performance of the rebuilt SUERC single-stage accelerator mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Shanks, Richard P.; Ascough, Philippa L.; Dougans, Andrew; Gallacher, Paul; Gulliver, Pauline; Rood, Dylan H.; Xu, Sheng; Freeman, Stewart P.H.T.

    2015-10-15

    The SUERC bipolar single-stage accelerator mass spectrometer (SSAMS) has been dismantled and rebuilt to accommodate an additional rotatable pre-accelerator electrostatic spherical analyser (ESA) and a second ion source injector. This is for the attachment of an experimental positive-ion electron cyclotron resonance (ECR) ion source in addition to a Cs-sputter source. The ESA significantly suppresses oxygen interference to radiocarbon detection, and remaining measurement interference is now thought to be from {sup 13}C injected as {sup 13}CH molecule scattering off the plates of a second original pre-detector ESA.

  14. Surface modifications of stainless steel to minimise contamination in mass spectrometers

    Science.gov (United States)

    Abda, J.; Douce, D.; Jones, G.; Skeldon, P.; Thompson, G. E.

    2015-12-01

    The effect of electrochemically grown and vapour deposited coatings on the build-up of contamination on stainless steel surfaces in the electrospray ionisation source of a mass spectrometer is investigated, together with their influence on the robustness of the instrument response. Quantification of the contamination build-up on flat samples, using white light interferometry, allowed the identification of the most beneficial treatments. Coating with electrochemically-grown anodic oxide and cathodic oxide films and amorphous carbon films doped with silicon or nitrogen resulted in reduced contamination compared with the uncoated stainless steel surface, and provided improved robustness of the instrument response.

  15. Onsets of nuclear deformation from measurements with the Isoltrap mass spectrometer

    CERN Document Server

    Naimi, Sarah

    Mass measurements provide important information concerning nuclear structure. This work presents results from the pioneering Penning trap spectrometer ISOLTRAP at CERN-ISOLDE. High-precision mass measurements of neutron-rich manganese ($^{58−66}$Mn) and krypton isotopes ($^{96,97}$Kr) are presented, of which the $^{66}$Mn and $^{96,97}$Kr masses are measured for the first time. In particular, the mass of $^{97}$Kr was measured using the preparation trap and required the definition of a new fit function. In the case of the manganese isotopes, the N = 40 shell closure is addressed. The two-neutron-separation energies calculated from the new masses show no shell closure at N = 40 but give an estimation of the proton-neutron interaction (around 0.5 MeV) responsible for the increase of collectivity and nuclear deformation in this mass region. The new krypton masses show behavior in sharp contrast with heavier neighbors where sudden and intense deformation is present, interpreted as the establishment of a nuclea...

  16. Detection of Gelatin Adulteration in Traditional Chinese Medicine: Analysis of Deer-Horn Glue by Rapid-Resolution Liquid Chromatography-Triple Quadrupole Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jia Chen

    2015-01-01

    Full Text Available Simultaneous identification of donkey-hide gelatin and bovine-hide gelatin in deer-horn glue was established by rapid-resolution liquid chromatography-triple quadrupole mass spectrometry. Water containing 1% NH4HCO3 was used for sample dissolution and trypsin was used for hydrolysis of the gelatins. After separation by a SB-C18 reversed-phase analytical column, collagen marker peptides were detected by mass spectrometry in positive electrospray ionization mode with multiple reaction monitoring. The method was specific, precise and reliable, and suitable for detection of adulterants derived from donkey-hide gelatin and bovine-hide gelatin in deer-horn glue.

  17. High-accuracy mass determination of unstable nuclei with a Penning trap mass spectrometer

    CERN Multimedia

    2002-01-01

    The mass of a nucleus is its most fundamental property. A systematic study of nuclear masses as a function of neutron and proton number allows the observation of collective and single-particle effects in nuclear structure. Accurate mass data are the most basic test of nuclear models and are essential for their improvement. This is especially important for the astrophysical study of nuclear synthesis. In order to achieve the required high accuracy, the mass of ions captured in a Penning trap is determined via their cyclotron frequency $ \

  18. A new approach for simultaneous screening and quantification of toxic pyrrolizidine alkaloids in some potential pyrrolizidine alkaloid-containing plants by using ultra performance liquid chromatography-tandem quadrupole mass spectrometry.

    Science.gov (United States)

    Zhou, Yan; Li, Na; Choi, Franky Fung-Kei; Qiao, Chun-Feng; Song, Jing-Zheng; Li, Song-Lin; Liu, Xin; Cai, Zong-Wei; Fu, Peter P; Lin, Ge; Xu, Hong-Xi

    2010-11-29

    A rapid, but sensitive and selective method for simultaneous screening and quantification of toxic pyrrolizidine alkaloids (PAs) by ultra performance liquid-chromatography (UPLC) coupled with tandem mass spectrometry (MS/MS) on a tandem quadrupole mass spectrometer (TQ-MS) is described. This was accomplished by incorporating the precursor ion scan (PIS) acquisition and multiple reaction monitoring (MRM) acquisition in the same UPLC-MS/MS run. Notably, the developed PIS approach for detecting two pairs of characteristic product ions at m/z 120/138 or 168/150, allowed specific identification of toxic retronecine and otonecine types PAs. This PIS method is highly sensitive with over 10-fold sensitivity improvement upon previously published LC-MS method. Moreover, this new approach is suitable for high sample throughput and was applied to the screening and quantifying toxic PAs in 22 samples collected from seven Parasenecio species and four Senecio species. In addition, coupling the MRM with PIS approach generated quantitative results equivalent to those obtained by conventional MRM-only approach. This coupled MRM with PIS approach could provide both qualitative and quantitative results without the need of repetitive analyses.

  19. Atmospheric pressure gas chromatography coupled to quadrupole-time of flight mass spectrometry as a tool for identification of volatile migrants from autoadhesive labels used for direct food contact.

    Science.gov (United States)

    Canellas, Elena; Vera, Paula; Nerín, Cristina

    2014-11-01

    Pressure-sensitive adhesives (PSA) are used to manufacture labels that are applied directly on the food. These adhesives could contain not only intentionally added compounds (IAS) to the adhesive formula but also non-intentionally added substances (NIAS), due to the impurities from the raw materials used, decomposition of the initial components or from chemical interactions between them. These compounds could migrate to the food and contaminate it. In this study, gas chromatography coupled with mass spectrometry (GC-MS/Q) and atmospheric pressure gas chromatography coupled to a quadrupole hyphenated to a time of flight mass spectrometer (APGC-MS/Q-TOF) have been used for identification of unknown compounds and NIAS coming from a PSA. Seven compounds were identified by GC-MS/Q, and other eight compounds remained initially unknown. The structure of these eight new compounds was elucidated by working with the spectra obtained by APGC-MS/Q-TOF. Finally, two different migration studies were carried out. The first one with Tenax as solid food simulant in contact with the paper label containing the adhesive and the second one with isooctane filled in a natural pork intestine where the label containing the adhesive was applied on the external side. The results are shown and discussed.

  20. Evaluation of the absorption of methotrexate on cells and its cytotoxicity assay by using an integrated microfluidic device coupled to a mass spectrometer.

    Science.gov (United States)

    Gao, Dan; Li, Haifang; Wang, Niejun; Lin, Jin-Ming

    2012-11-06

    An integrated microfluidic device was developed for high-throughput drug screening with an online electrospray ionization quadrupole time-of-flight mass spectrometer (ESI-Q-TOF MS). The multiple gradient generator followed by an array of microscale cell culture chambers and on-chip solid-phase extraction (SPE) columns for sample pretreatment prior to mass analysis was integrated in the device which was fabricated in one single step. By using the combination system, the process for characterization of drug absorption and evaluation of cytotoxicity could be simultaneously realized. To validate the feasibility, the absorption of methotrexate and its effects on HepG2 and Caco-2 cells were investigated. With the increasing concentration of drugs, the percentage of apoptotic cells appeared in a dose-dependent fashion. By comparison with the results obtained from ESI-Q-TOF MS analysis and cytotoxicity assay, we found that higher intracellular drug concentration resulted in increased cell cytotoxicity. The technique presented herein provides an easy protocol to screen drugs rapidly with low drug consumption, high throughput, and high sensitivity.

  1. Networking mass spectrometer data systems for improved productivity and electronic archiving of data.

    Science.gov (United States)

    Hayward, M J; Robandt, P V; Meek, J T; Thomson, M L

    1993-09-01

    Several Finngan-MAT mass spectrometer data systems were networked together to achieve the following two primary objectives: (1) to allow access to mass spectrometry data and data processing functions from remote locations without affecting simultaneous data acquisition at the instruments, and (2) to electronically archive mass spectrometry data at a central location on a high-capacity, fast-access device that allows rapid retrieval of archived data for all data processing operations at all locations. UNIX workstations, IBM PC/AT-compatible computers, and Data General Nova minicomputers were connected via Ethernet interfaces to allow rapid data transfer among all systems as well as X-Windows access to UNIX-based systems. Bridging techniques were used to isolate possible high-traffic areas of the network and to enable security measures for adequate protection of files. Additionally, serial connections were made through a Northern Telecom phone system to provide remote terminal access to the Data General Nova-based systems. Use of these connectivity techniques significantly improved productivity by allowing retrieval, processing, and printing of data from remote locations, such as office areas, without affecting data acquisition, processing, and printing performed simultaneously at the instruments. For archival purposes, data files are electronically stored on high-capacity magneto-optical disks for rapid retrieval. A highcapacity fixed disk is also available for centralized temporary data file storage. A Digital Equipment Corporation DECstation 2100 UNIX workstation was used as the file server for centralized data storage while being simultaneously utilized as the data system computer for one of the mass spectrometers. Utilization of this UNIX-based file server system in conjunction with Ethernet connectivity techniques provides a centralized, rapid-access, high-capacity, cost- and space-efficient method for electronic archival of mass spectrometry raw data recorded

  2. Carbon cluster mass calibration at the double Penning trap mass spectrometer TRIGA-TRAP

    Energy Technology Data Exchange (ETDEWEB)

    Smorra, Christian [Physikalisches Institut, Universitaet Heidelberg (Germany); Institut fuer Kernchemie, Universitaet Mainz (Germany); Blaum, Klaus [Physikalisches Institut, Universitaet Heidelberg (Germany); Max-Planck Institut fuer Kernphysik, Heidelberg (Germany); Eberhardt, Klaus [Institut fuer Kernchemie, Universitaet Mainz (Germany); Eibach, Martin; Ketelaer, Jens; Ketter, Jochen; Knuth, Konstantin [Institut fuer Physik, Universitaet Mainz (Germany); Herfurth, Frank [GSI, Helmholtzzentrum fuer Schwerionenforschung GmbH, Darmstadt (Germany); Nagy, Szilard [Max-Planck Institut fuer Kernphysik, Heidelberg (Germany)

    2009-07-01

    TRIGA-TRAP is a facility which aims for mass measurements on neutron-rich short-lived fission products and actinides with relative mass uncertainties of 10{sup -7} and below. To this end the cyclotron frequency of a stored ion in a Penning trap is determined. In high-precision mass spectrometry the investigation of systematic errors is of utmost importance. In order to demonstrate the accuracy of the measured values, various carbon cluster ions have been used in cross reference measurements. The results are presented and the accuracy limit of TRIGA-TRAP is discussed.

  3. Helium Mass Spectrometer Leak Detection: A Method to Quantify Total Measurement Uncertainty

    Science.gov (United States)

    Mather, Janice L.; Taylor, Shawn C.

    2015-01-01

    In applications where leak rates of components or systems are evaluated against a leak rate requirement, the uncertainty of the measured leak rate must be included in the reported result. However, in the helium mass spectrometer leak detection method, the sensitivity, or resolution, of the instrument is often the only component of the total measurement uncertainty noted when reporting results. To address this shortfall, a measurement uncertainty analysis method was developed that includes the leak detector unit's resolution, repeatability, hysteresis, and drift, along with the uncertainty associated with the calibration standard. In a step-wise process, the method identifies the bias and precision components of the calibration standard, the measurement correction factor (K-factor), and the leak detector unit. Together these individual contributions to error are combined and the total measurement uncertainty is determined using the root-sum-square method. It was found that the precision component contributes more to the total uncertainty than the bias component, but the bias component is not insignificant. For helium mass spectrometer leak rate tests where unit sensitivity alone is not enough, a thorough evaluation of the measurement uncertainty such as the one presented herein should be performed and reported along with the leak rate value.

  4. MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission: results and performance

    Science.gov (United States)

    Buch, A.; Pinnick, V. T.; Szopa, C.; Grand, N.; Humeau, O.; van Amerom, F. H.; Danell, R.; Freissinet, C.; Brinckerhoff, W.; Gonnsen, Z.; Mahaffy, P. R.; Coll, P.; Raulin, F.; Goesmann, F.

    2015-10-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquiring samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular and chiral) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis/chemical derivatization gas chromatography (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide information on elemental and molecular makeup, polarity, chirality and isotopic patterns of analyte species. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatographymass spectrometry (GC-MS) mode of operation.

  5. Development of a portable time-of-flight membrane inlet mass spectrometer for environmental analysis

    Science.gov (United States)

    White, A. J.; Blamire, M. G.; Corlett, C. A.; Griffiths, B. W.; Martin, D. M.; Spencer, S. B.; Mullock, S. J.

    1998-02-01

    The benefits of on-site analysis of environmental pollutants are well known, with such techniques increasing sample throughput and reducing the overall cost of pollution level monitoring. This article describes a transportable time-of-flight (TOF) mass spectrometer, based upon a converging, annular TOF (CAT) arrangement. The instrument, the transportable CAT or T-CAT is battery powered and self-contained. The vacuum chamber is never vented and is kept at a very low pressure, even during analysis. Sample gases are admitted to the mass spectrometer via a membrane inlet system. Data collection and analysis are accomplished via a portable PC. The T-CAT is capable of detection limits approaching those of more conventional, nonportable design. The device shows reasonable linearity over wide concentration ranges. Initial results indicate that the T-CAT will be capable of use in a wide range of applications, particularly for environmental monitoring. This article describes the features of the T-CAT, and presents initial results from the membrane inlet/T-CAT system.

  6. Numerical investigation of interface region flows in mass spectrometers: neutral gas transport

    Energy Technology Data Exchange (ETDEWEB)

    Jugroot, Manish [Institute for Aerospace Studies, University of Toronto, 4925 Dufferin Street, Toronto, Ontario, M3H 5T6 (Canada); Groth, Clinton P T [Institute for Aerospace Studies, University of Toronto, 4925 Dufferin Street, Toronto, Ontario, M3H 5T6 (Canada); Thomson, Bruce A [MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, L4K 4V8 (Canada); Baranov, Vladimir [MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, L4K 4V8 (Canada); Collings, Bruce A [MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, L4K 4V8 (Canada)

    2004-04-21

    The supersonic jet flows of neutral gas from atmospheric to near-vacuum conditions in the interface region of mass-spectrometer systems is investigated by continuum-based (fluid) numerical simulations. An enhanced understanding of the neutral gas transport is of paramount importance to fully understand flows in the interface region of mass spectrometers, for it is the neutral dynamics that governs and drives the ions from the high pressure ion source through the interface orifice towards the ion optics and detector subsystems. The key features and structure of the complex neutral gas flow are examined and the influence of large pressure differences imposed across the interface region, orifice geometry, and gas skimmer configuration used for flow control are assessed. The flow structure is shown to be that of a classical under-expanded free jet for 'skimmer-absent' cases and very good agreement between the numerical predictions and empirical and experimental values is demonstrated. For the 'skimmer-present' cases, the shock structure downstream of the orifice and skimmer is identified and fully described and its influences on the flow skimming and focusing processes are discussed.

  7. Super-Atmospheric Pressure Ion Sources: Application and Coupling to API Mass Spectrometer.

    Science.gov (United States)

    Chen, Lee Chuin; Rahman, Md Matiur; Hiraoka, Kenzo

    2014-01-01

    Pressurizing the ionization source to gas pressure greater than atmospheric pressure is a new tactic aimed at further improving the performance of atmospheric pressure ionization (API) sources. In principle, all API sources, such as ESI, APCI and AP-MALDI, can be operated at pressure higher than 1 atm if suitable vacuum interface is available. The gas pressure in the ion source can have different role for different ionization. For example, in the case of ESI, stable electrospray could be sustained for high surface tension liquid (e.g., pure water) under super-atmospheric pressure, owing to the absence of electric discharge. Even for nanoESI, which is known to work well with aqueous solution, its stability and sensitivity were found to be enhanced, particularly in the negative mode when the ion source was pressurized. For the gas phase ionization like APCI, measurement of gaseous compound also showed an increase in ion intensity with the ion source pressure until an optimum pressure at around 4-5 atm. The enhancement was due to the increased collision frequency among reactant ion and analyte that promoted the ion/molecule reaction and a higher intake rate of gas to the mass spectrometer. Because the design of vacuum interface for API instrument is based on the upstream pressure of 1 atm, some coupling aspects need to be considered when connecting the high pressure ion source to the mass spectrometer. Several coupling strategies are discussed in this paper.

  8. Broad-band FT-ICR detection at the Penning trap mass spectrometer TRIGA-TRAP

    Energy Technology Data Exchange (ETDEWEB)

    Knuth, Konstantin; Eibach, Martin; Ketelaer, Jens; Ketter, Jochen; Sturm, Sven [Institut fuer Physik, Universitaet Mainz (Germany); Blaum, Klaus [Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany); Physikalisches Institut, Universitaet Heidelberg Heidelberg (Germany); Block, Michael; Herfurth, Frank [GSI, Helmholtzzentrum fuer Schwerionenforschung, Darmstadt (Germany); Eberhardt, Klaus [Institut fuer Kernchemie, Universitaet Mainz (Germany); Nagy, Szilard [Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany); Repp, Julia [Institut fuer Physik, Universitaet Mainz (Germany); Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany); Smorra, Christian [Physikalisches Institut, Universitaet Heidelberg Heidelberg (Germany); Institut fuer Kernchemie, Universitaet Mainz (Germany); Ulmer, Stefan [Institut fuer Physik, Universitaet Mainz (Germany); Physikalisches Institut, Universitaet Heidelberg Heidelberg (Germany)

    2009-07-01

    The double Penning trap mass spectrometer TRIGA-TRAP will perform high-precision mass measurements on exotic neutron-rich nuclides, which are produced via neutron-induced fission of actinide targets at the research reactor TRIGA Mainz. In order to determine which ion species are present in the ion bunch delivered to the Penning trap system, a non-destructive ion detection technique will be implemented in the cylindrical purification trap. This so called broad-band Fourier transform ion cyclotron resonance (FT-ICR) detection technique is based on the detection of image currents, induced by the ions in the trap electrodes. To this end, a new cryogenic low-noise broad-band amplifier is being designed and tested. With this system the identification of contaminations will be possible without the need to eject ions from the trap as usually done at other facilities. The setup as well as its present status are presented.

  9. Manifold and method of batch measurement of Hg-196 concentration using a mass spectrometer

    Science.gov (United States)

    Grossman, M.W.; Evans, R.

    1991-11-26

    A sample manifold and method of its use has been developed so that milligram quantities of mercury can be analyzed mass spectroscopically to determine the [sup 196]Hg concentration to less than 0.02 atomic percent. Using natural mercury as a standard, accuracy of [+-]0.002 atomic percent can be obtained. The mass spectrometer preferably used is a commercially available GC/MS manufactured by Hewlett Packard. A novel sample manifold is contained within an oven allowing flow rate control of Hg into the MS. Another part of the manifold connects to an auxiliary pumping system which facilitates rapid clean up of residual Hg in the manifold. Sample cycle time is about 1 hour. 8 figures.

  10. Feasibility of a Fieldable Mass Spectrometer FY 2015 Year-end Report

    Energy Technology Data Exchange (ETDEWEB)

    Barinaga, Charles J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hager, George J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hoegg, Edward D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Carman, April J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hart, Garret L. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2015-10-01

    Currently, the International Atomic Energy Agency (IAEA) monitors the production of enriched uranium hexafluoride (UF6) at declared facilities by collecting a few grams of product in sample tubes that are then sent to central laboratories for processing and isotope ratio analysis by thermal ionization mass spectrometry. Analysis of results may not be available for some time after collection. In addition, new shipping regulations will make it more difficult to transport this amount of UF6 to a laboratory. The IAEA is interested in an isotope ratio technique for uranium in UF6 that can be moved to and operated at the enrichment facility itself. This report covers the tasks and activities of the Feasibility of a Fieldable Mass Spectrometer Project for FY 2015, which investigates the feasibility of an in-field isotope ratio technique— the forward deployment of a technique to the non-laboratory situation of a protected room with power and heat at the facility of interest.

  11. Spatial variation of chemical composition and sources of submicron aerosol in Zurich: factor analysis of mobile aerosol mass spectrometer data

    Directory of Open Access Journals (Sweden)

    C. Mohr

    2011-04-01

    Full Text Available Mobile measurements of PM1 (PM with an aerodynamic diameter D<1 μm chemical composition using a quadrupole aerosol mass spectrometer and a multi-angle absorption photometer were performed using the PSI mobile laboratory during winter 2007/2008 and December 2008 in the metropolitan area of Zurich, Switzerland. Positive matrix factorization (PMF applied to the organic fraction of PM1 yielded 3 factors: Hydrocarbon-like organic aerosol (HOA related to traffic emissions; organic aerosol from wood burning for domestic heating purposes (WBOA; and oxygenated organic aerosol (OOA, assigned to secondary organic aerosol formed by oxidation of volatile precursors. The spatial variation of the chemical composition of PM1 shows a uniform distribution throughout the city: for primary emissions, road traffic is important along major roads (varying between 7 and 14% of PM1 for different sites within the city, but overall, domestic wood burning is more important for the organic aerosol concentrations in Zurich during winter time (varying between 8–15% of PM1 for different sites within the city. OOA makes up the largest fraction of organic aerosol (44% on average. A new method, based on simultaneous on-road mobile and stationary background measurements and using the ratio of on-road sulfate to stationary sulfate to correct for small-scale dynamic effects, allows for the separation of PM1 emitted or produced locally and the PM1 from the regional background. It could be shown that especially during thermal inversions over the Swiss plateau, regional background concentrations contribute substantially to particulate number concentrations (60% on average as well as to the concentrations of PM1 components (on average 60% for black carbon and HOA, over 97% for WBOA and OOA, and more than 94% for the measured inorganic components in downtown Zurich. The results emphasize, on

  12. Development of analytically capable time-of-flight mass spectrometer with continuous ion introduction

    Science.gov (United States)

    Hárs, György; Dobos, Gábor

    2010-03-01

    The present article describes the results and findings explored in the course of the development of the analytically capable prototype of continuous time-of-flight (CTOF) mass spectrometer. Currently marketed pulsed TOF (PTOF) instruments use ion introduction with a 10 ns or so pulse width, followed by a waiting period roughly 100 μs. Accordingly, the sample is under excitation in 10-4 part of the total measuring time. This very low duty cycle severely limits the sensitivity of the PTOF method. A possible approach to deal with this problem is to use linear sinusoidal dual modulation technique (CTOF) as described in this article. This way the sensitivity of the method is increased, due to the 50% duty cycle of the excitation. All other types of TOF spectrometer use secondary electron multiplier (SEM) for detection, which unfortunately discriminates in amplification in favor of the lighter ions. This discrimination effect is especially undesirable in a mass spectrometric method, which targets high mass range. In CTOF method, SEM is replaced with Faraday cup detector, thus eliminating the mass discrimination effect. Omitting SEM is made possible by the high ion intensity and the very slow ion detection with some hundred hertz detection bandwidth. The electrometer electronics of the Faraday cup detector operates with amplification 1010 V/A. The primary ion beam is highly monoenergetic due to the construction of the ion gun, which made possible to omit any electrostatic mirror configuration for bunching the ions. The measurement is controlled by a personal computer and the intelligent signal generator Type Tabor WW 2571, which uses the direct digital synthesis technique for making arbitrary wave forms. The data are collected by a Labjack interface board, and the fast Fourier transformation is performed by the software. Noble gas mixture has been used to test the analytical capabilities of the prototype setup. Measurement presented proves the results of the mathematical

  13. Development of analytically capable time-of-flight mass spectrometer with continuous ion introduction.

    Science.gov (United States)

    Hárs, György; Dobos, Gábor

    2010-03-01

    The present article describes the results and findings explored in the course of the development of the analytically capable prototype of continuous time-of-flight (CTOF) mass spectrometer. Currently marketed pulsed TOF (PTOF) instruments use ion introduction with a 10 ns or so pulse width, followed by a waiting period roughly 100 micros. Accordingly, the sample is under excitation in 10(-4) part of the total measuring time. This very low duty cycle severely limits the sensitivity of the PTOF method. A possible approach to deal with this problem is to use linear sinusoidal dual modulation technique (CTOF) as described in this article. This way the sensitivity of the method is increased, due to the 50% duty cycle of the excitation. All other types of TOF spectrometer use secondary electron multiplier (SEM) for detection, which unfortunately discriminates in amplification in favor of the lighter ions. This discrimination effect is especially undesirable in a mass spectrometric method, which targets high mass range. In CTOF method, SEM is replaced with Faraday cup detector, thus eliminating the mass discrimination effect. Omitting SEM is made possible by the high ion intensity and the very slow ion detection with some hundred hertz detection bandwidth. The electrometer electronics of the Faraday cup detector operates with amplification 10(10) V/A. The primary ion beam is highly monoenergetic due to the construction of the ion gun, which made possible to omit any electrostatic mirror configuration for bunching the ions. The measurement is controlled by a personal computer and the intelligent signal generator Type Tabor WW 2571, which uses the direct digital synthesis technique for making arbitrary wave forms. The data are collected by a Labjack interface board, and the fast Fourier transformation is performed by the software. Noble gas mixture has been used to test the analytical capabilities of the prototype setup. Measurement presented proves the results of the

  14. 160 keV {sup 26}Al-AMS with a single-stage accelerator mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Shanks, Richard P.; Freeman, Stewart P.H.T.

    2015-10-15

    Proof-of-principle {sup 26}Al-AMS analysis is achieved with a single-stage accelerator mass spectrometer (SSAMS) utilising very low ion energy. The SSAMS operates by discriminating against atomic isobar interference in a negative ion source and suppressing molecules with thick gas stripper. Resulting 1+ ions counting is with a surface barrier detector. The NEC designed SSAMS for {sup 14}C analysis is a popular model accelerator mass spectrometer and the developed further capability might be a significant addition to established {sup 26}Al-AMS capacity. Measurements at these energies should also be sufficient for alternative {sup 26}Al positive-ion mass spectrometry (PIMS).

  15. Highly miniaturized laser ablation time-of-flight mass spectrometer for a planetary rover

    Science.gov (United States)

    Rohner, Urs; Whitby, James A.; Wurz, Peter; Barabash, Stas

    2004-05-01

    We report the development and testing of a highly miniaturized mass spectrometer and ion source intended to be deployed on an airless planetary surface to measure the elemental and isotopic composition of solids, e.g., rocks and soils. Our design concentrates at this stage on the proposed BepiColombo mission to the planet Mercury. The mass analyzer is a novel combination of an electrostatic analyzer and a reflectron time-of-flight design. The ion source utilizes a laser induced plasma, which is directly coupled into the mass analyzer. Laser ablation gives high spatial resolution and avoids the need for sample preparation. Our prototype instrument has a demonstrated mass resolution m/Δm full width at half maximum in excess of 180 and a predicted dynamic range of better than five orders of magnitude. We estimate that a flight instrument would have a mass of 280 g (including laser and all electronics), a volume of 84 cm3, and could operate on 3 W power.

  16. Advanced Laser Architecture for Two-Step Laser Tandem Mass Spectrometer

    Science.gov (United States)

    Fahey, Molly E.; Li, Steven X.; Yu, Anthony W.; Getty, Stephanie A.

    2016-01-01

    Future astrobiology missions will focus on planets with significant astrochemical or potential astrobiological features, such as small, primitive bodies and the icy moons of the outer planets that may host diverse organic compounds. These missions require advanced instrument techniques to fully and unambiguously characterize the composition of surface and dust materials. Laser desorptionionization mass spectrometry (LDMS) is an emerging instrument technology for in situ mass analysis of non-volatile sample composition. A recent Goddard LDMS advancement is the two-step laser tandem mass spectrometer (L2MS) instrument to address the need for future flight instrumentation to deconvolve complex organic signatures. The L2MS prototype uses a resonance enhanced multi-photon laser ionization mechanism to selectively detect aromatic species from a more complex sample. By neglecting the aliphatic and inorganic mineral signatures in the two-step mass spectrum, the L2MS approach can provide both mass assignments and clues to structural information for an in situ investigation of non-volatile sample composition. In this paper we will describe our development effort on a new laser architecture that is based on the previously flown Lunar Orbiter Laser Altimeter (LOLA) laser transmitter for the L2MS instrument. The laser provides two discrete midinfrared wavelengths (2.8 m and 3.4 m) using monolithic optical parametric oscillators and ultraviolet (UV) wavelength (266 nm) on a single laser bench with a straightforward development path toward flight readiness.

  17. Mass measurements on short-lived Cd and Ag nuclides at the online mass spectrometer ISOLTRAP

    Energy Technology Data Exchange (ETDEWEB)

    Breitenfeldt, Martin

    2009-07-03

    In the present work, mass determinations of the eleven neutron-deficient nuclides {sup 99-109}Cd, of ten neutron-rich silver nuclides {sup 112,114-121,123}Ag, and seven neutron-rich cadmium nuclides {sup 114,120,122-124,126,128}Cd are reported. Due to the clean production of the neutron-deficient nuclides it was possible to reduce the experimental uncertainties down to 2 keV, whereas the measurements of neutron-rich nuclides were hampered by the presence of contaminations from more stable In and Cs nuclides. In the case of {sup 99}Cd and {sup 123}Ag the masses were determined for the first time and for the other nuclides the mass uncertainties could be reduced by up to a factor of 50 as in the case of {sup 100}Cd. In the case of a potential isomeric mixture as for {sup 115,117,119}Ag and {sup 123}Cd, where no assignment to either the ground state or the excited state was possible, the experimental results were adjusted accordingly. Afterwards all results were included in the framework of the atomic-mass evaluation and thus linked and compared with other experimental data. In the case of a potential isomeric mixture as for {sup 115,117,119}Ag and {sup 123}Cd, where no assignment to either the ground state or the excited state was possible, the experimental results were adjusted accordingly. Afterwards all results were included in the framework of the atomic-mass evaluation and thus linked and compared with other experimental data. In the case of the neutron-deficient Cd nuclides a conflict between the mass values obtained in the present work and those published by the JYFLTRAP group [EEH{sup +}] could be solved by performing an atomic-mass evaluation. Thus, it was revealed that reason for the conflict was a different value of the JYFLTRAP reference mass {sup 96}Mo. Furthermore, a reduction of the mass uncertainty and a slight increase of the mass of {sup 100}In were obtained. These mass measurements are an important step towards an understanding of the physics of

  18. Profiling the indole alkaloids in yohimbe bark with ultra-performance liquid chromatography coupled with ion mobility quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Sun, Jianghao; Baker, Andrew; Chen, Pei

    2011-09-30

    An ultra-performance liquid chromatography/ion mobility quadrupole time-of-flight mass spectrometry (UPLC/IM-QTOF-MS) method was developed for profiling the indole alkaloids in yohimbe bark. Many indole alkaloids with the yohimbine or ajmalicine core structure, plus methylated, oxidized and reduced species, were characterized. Common fragments and mass differences are described. It was shown that the use of IMS could provide another molecular descriptor, i.e. molecular shape by rotationally averaged collision cross-section; this is of great value for identification of constituents when reference materials are usually not available. Using the combination of high resolution (~40000) accurate mass measurement with time-aligned parallel (TAP) fragmentation, MS(E) (where E represents collision energy), ion mobility mass spectrometry (IMS) and UPLC chromatography, a total 55 indole alkaloids were characterized and a few new indole alkaloids are reported for the first time.

  19. Identification of metabolites of Radix Paeoniae Alba extract in rat bile, plasma and urine by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Zheng-Wei Chen; Ling Tong; Shu-Ming Li; Dong-Xiang Li; Ying Zhang; Shui-Ping Zhou; Yong-Hong Zhu; He Sun

    2014-01-01

    Ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF/MS) was developed to identify the absorbed parent components and metabolites in rat bile, plasma and urine after oral administration of Radix Paeoniae Alba extract (RPAE). A total of 65 compounds were detected in rat bile, plasma and urine samples, including 11 parent compounds and 54 metabolites. The results indicated that glucuronidation, hydroxylation and methylation were the major metabolic pathways of the components of RPAE. Furthermore, the results of this work demonstrated that UPLC-Q-TOF/MS combined with MetaboLynx™ software and mass defect filtering (MDF) could provide unique high throughput capabilities for drug metabolism study, with excellent MS mass accuracy and enhanced MSE data acquisition. With the MSE technique, both precursor and fragment mass spectra can be simultaneously acquired by alternating between high and low collision energy during a single chromatographic run.

  20. Mass measurements on short-lived Cd and Ag nuclides at the online mass spectrometer ISOLTRAP

    Energy Technology Data Exchange (ETDEWEB)

    Breitenfeldt, Martin

    2009-07-03

    In the present work, mass determinations of the eleven neutron-deficient nuclides {sup 99-109}Cd, of ten neutron-rich silver nuclides {sup 112,114-121,123}Ag, and seven neutron-rich cadmium nuclides {sup 114,120,122-124,126,128}Cd are reported. Due to the clean production of the neutron-deficient nuclides it was possible to reduce the experimental uncertainties down to 2 keV, whereas the measurements of neutron-rich nuclides were hampered by the presence of contaminations from more stable In and Cs nuclides. In the case of {sup 99}Cd and {sup 123}Ag the masses were determined for the first time and for the other nuclides the mass uncertainties could be reduced by up to a factor of 50 as in the case of {sup 100}Cd. In the case of a potential isomeric mixture as for {sup 115,117,119}Ag and {sup 123}Cd, where no assignment to either the ground state or the excited state was possible, the experimental results were adjusted accordingly. Afterwards all results were included in the framework of the atomic-mass evaluation and thus linked and compared with other experimental data. In the case of a potential isomeric mixture as for {sup 115,117,119}Ag and {sup 123}Cd, where no assignment to either the ground state or the excited state was possible, the experimental results were adjusted accordingly. Afterwards all results were included in the framework of the atomic-mass evaluation and thus linked and compared with other experimental data. In the case of the neutron-deficient Cd nuclides a conflict between the mass values obtained in the present work and those published by the JYFLTRAP group [EEH{sup +}] could be solved by performing an atomic-mass evaluation. Thus, it was revealed that reason for the conflict was a different value of the JYFLTRAP reference mass {sup 96}Mo. Furthermore, a reduction of the mass uncertainty and a slight increase of the mass of {sup 100}In were obtained. These mass measurements are an important step towards an understanding of the physics of

  1. Design of Portable Mass Spectrometers with Handheld Probes: Aspects of the Sampling and Miniature Pumping Systems

    Science.gov (United States)

    Chen, Chien-Hsun; Chen, Tsung-Chi; Zhou, Xiaoyu; Kline-Schoder, Robert; Sorensen, Paul; Cooks, R. Graham; Ouyang, Zheng

    2015-02-01

    Miniature mass spectrometry analytical systems of backpack configuration fitted with sampling probes could potentially be of significant interest for in-field, real-time chemical analysis. In this study, various configurations were explored in which a long narrow tube was used to connect the turbo and backing pumps used to create and maintain vacuum. Also, for the first time we introduced two new types of pumps for miniature mass spectrometers, the Creare 130 g drag pump and Creare 350 g scroll backing pump. These pumps, along with another Creare 550 turbo pump and the commercially available Pfeiffer HiPace 10 turbo and KnF diaphragm backing pumps, were tested with the backpack configurations. The system performance, especially the scan time, was characterized when used with a discontinuous atmospheric pressure interface (DAPI) for ion introduction. The pumping performance in the pressure region above 1 mtorr is critical for DAPI operation. The 550 g turbo pump was shown to have a relatively higher pumping speed above 1 mtorr and gave a scan time of 300 ms, almost half the value obtained with the larger, heavier HiPace 10 often used with miniature mass spectrometers. The 350 g scroll pump was also found to be an improvement over the diaphragm pumps generally used as backing pumps. With a coaxial low temperature plasma ion source, direct analysis of low volatility compounds glass slides was demonstrated, including 1 ng DNP (2,4-Dinitrophenol) and 10 ng TNT (2,4,6-trinitrotoluene) with Creare 550 g turbo pump as well as 10 ng cocaine and 20 ng DNP with Creare 130 g drag pump.

  2. Performance of the MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission

    Science.gov (United States)

    Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Grand, Noël; Freissinet, Caroline; Danell, Ryan; van Ameron, Friso; Arevalo, Ricardo; Brinckerhoff, William; Raulin, François; Mahaffy, Paul; Goesmann, Fred

    2015-04-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquir-ing samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis gas chromatograph (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide in-formation on elemental and molecular makeup, po-larity, chirality and isotopic patterns of analyte spe-cies. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatography-mass spec-trometry (GC-MS) mode of operation. Both instruments have been tested separately first and have been coupled in order to test the efficiency of the future MOMA GC-MS instrument. The main objective of the second step has been to test the quantitative response of both instruments while they are coupled and to characterize the combined instrument detection limit for several compounds. A final experiment has been done in order to test the feasibility of the separation and detection of a mixture contained in a soil sample introduced in the MOMA oven.

  3. Identification of unknown pesticides in fruits using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Imazalil as a case study of quantification.

    Science.gov (United States)

    Picó, Yolanda; la Farré, Marinel; Soler, Carla; Barceló, Damià

    2007-12-28

    Ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QqTOF-MS) is an emerging technique offering more rapid and efficient separation, as well as the possibility to obtain accurate mass measurement and tandem mass spectrometry (MS/MS). This paper deals with the use of UPLC-QqTOF-MS to identify the pesticide residues present in complex pear extracts. Carbendazim, imazalil, and ethoxyquin were successfully identified because of the accurate mass determination of their protonated molecule and their major fragments in the product ion mass spectra. A few plastic and latex additives were also found, most of them probably coming from the packaging transfer to the fruits. The potential of the UPLC-QqTOF-MS and UPLC-QqTOF-MS/MS techniques as a quantification tool is also discussed taking imazalil as example. For quantification, calibration curves were linear over a dynamic range of 2 orders of magnitude, whereas higher calibration ranges are better adjusted to polynomial curves of second and third order. Quantification using different mass windows was also assessed. Accurate quantification required mass windows as wide as 20 mDa, narrower mass windows of 5 mDa provided erroneous quantification, probably because the low ion abundance. The mean recoveries and percentage relative standard deviation (RSD) of 35 determinations for imazalil were 76% (13% RSD) by MS and 77% (14% RSD) by MS/MS. The theoretical limit of detection was 0.4 microg kg(-1), with a validated limit of quantification of 2 microg kg(-1). The quantitative data obtained using UPLC-QqTOF-MS were compared with those obtained using conventional liquid chromatography (LC)-MS/MS with a triple quadrupole (QqQ). It was concluded that UPLC-QqTOF-MS might become a powerful analytical tool for both, unknown's identification and quantification of target pesticides.

  4. Structure Analysis and Ion Abundance in CID- MS- MS Spectra of Isomeric Oligosaccharides Using Quadrupole Time-of- flight Mass Spectrometry: Distinguishing between Isomeric Oligosaccharides

    Institute of Scientific and Technical Information of China (English)

    Tohru YAMAGAKI; Kazuo TACHIBANA

    2001-01-01

    @@ N - Linked oligosaccharide were analyzed by using electrospray ionization (ESI) quadrupole time - of- fight mass spectrometry(Q - Tof MS).The isomers showed the same MS and collisioninduced desociation(CID) MS - MS spectra in the m/z values because the sequence of the sugar residues was the same.But the relative ion abundance of the specific fragment ion was greatly different between the isomers.So, the isomeric oligosacchariedes were distinguished by using the ion abundance in their CID -MS - MS spectra.Discussing the ion abundance in accurate level, quantitative analysis of the mixtures of isomers were also performed.

  5. Nuclear structure research with the Penning-trap mass spectrometer ISOLTRAP at CERN

    Energy Technology Data Exchange (ETDEWEB)

    Neidherr, Dennis [Johannes Gutenberg-Universitaet, Mainz (Germany)

    2009-07-01

    At the double-Penning-trap mass spectrometer ISOLTRAP at ISOLDE/CERN the cyclotron frequency of short-lived radionuclides is measured in order to determine their mass with a relative uncertainty in the order of 10{sup -8} and below. This ground state property plays an important role in many fields of modern physics from nuclear-structure research to nuclear astrophysics and tests of the weak interaction of the Standard Model. An example for the first one is the evolution of the nuclear shape as a function of the number of neutrons and protons. In 2008 the masses of {sup 223-229}Rn and {sup 143-146}Xe were measured for the first time directly, whereas {sup 229}Rn was even discovered by our Penning trap based experiment. With this mass values one can study the proton-neutron interaction and therefore get information about the nuclear structure like collectivity, the onset of deformation or the geometrical shapes in atomic nuclei. The experimental results as well as the impact on the theoretical models will be presented.

  6. A high-resolution x-ray spectrometer for a kaon mass measurement

    Science.gov (United States)

    Phelan, Kevin; Suzuki, Ken; Zmeskal, Johann; Tortorella, Daniele; Bühler, Matthias; Hertrich, Theo

    2017-02-01

    The ASPECT consortium (Adaptable Spectrometer Enabled by Cryogenic Technology) is currently constructing a generalised cryogenic platform for cryogenic detector work which will be able to accommodate a wide range of sensors. The cryogenics system is based on a small mechanical cooler with a further adiabatic demagnetisation stage and will work with cryogenic detectors at sub-Kelvin temperatures. The commercial aim of the consortium is to produce a compact, user-friendly device with an emphasis on reliability and portability which can easily be transported for specialised on-site work, such as beam-lines or telescope facilities. The cryogenic detector platform will accommodate a specially developed cryogenic sensor, either a metallic magnetic calorimeter or a magnetic penetration-depth thermometer. The detectors will be designed to work in various temperatures regions with an emphasis on optimising the various detector resolutions for specific temperatures. One resolution target is of about 10 eV at the energies range typically created in kaonic atoms experiments (soft x-ray energies). A following step will see the introduction of continuous, high-power, sub-Kelvin cooling which will bring the cryogenic basis for a high resolution spectrometer system to the market. The scientific goal of the project will produce an experimental set-up optimised for kaon-mass measurements performing high-resolution x-ray spectroscopy on a beam-line provided foreseeably by the J-PARC (Tokai, Japan) or DAΦNE (Frascati, Italy) facilities.

  7. Mass spectra features of biomass burning boiler and coal burning boiler emitted particles by single particle aerosol mass spectrometer.

    Science.gov (United States)

    Xu, Jiao; Li, Mei; Shi, Guoliang; Wang, Haiting; Ma, Xian; Wu, Jianhui; Shi, Xurong; Feng, Yinchang

    2017-11-15

    In this study, single particle mass spectra signatures of both coal burning boiler and biomass burning boiler emitted particles were studied. Particle samples were suspended in clean Resuspension Chamber, and analyzed by ELPI and SPAMS simultaneously. The size distribution of BBB (biomass burning boiler sample) and CBB (coal burning boiler sample) are different, as BBB peaks at smaller size, and CBB peaks at larger size. Mass spectra signatures of two samples were studied by analyzing the average mass spectrum of each particle cluster extracted by ART-2a in different size ranges. In conclusion, BBB sample mostly consists of OC and EC containing particles, and a small fraction of K-rich particles in the size range of 0.2-0.5μm. In 0.5-1.0μm, BBB sample consists of EC, OC, K-rich and Al_Silicate containing particles; CBB sample consists of EC, ECOC containing particles, while Al_Silicate (including Al_Ca_Ti_Silicate, Al_Ti_Silicate, Al_Silicate) containing particles got higher fractions as size increase. The similarity of single particle mass spectrum signatures between two samples were studied by analyzing the dot product, results indicated that part of the single particle mass spectra of two samples in the same size range are similar, which bring challenge to the future source apportionment activity by using single particle aerosol mass spectrometer. Results of this study will provide physicochemical information of important sources which contribute to particle pollution, and will support source apportionment activities. Copyright © 2017. Published by Elsevier B.V.

  8. Electrospray Ionization/Ion Mobility Spectrometer/Cylindrical Ion Trap Mass Spectrometer System for In-Situ Detection of Organic Compounds

    Science.gov (United States)

    Kanik, I.; Johnson, P. V.; Beegle, L. W.; Cooks, R. G.; Laughlin, B. C.; Hill, H. H.

    2003-01-01

    The potential of an Electrospray Ionization/Ion Mobility Spectrometer/Cylindrical Ion Trap Mass Spectrometer (ESI/IMS/CIT-MS) as an analytical instrument for analyzing material extracted from rock and soil samples as part of a suite of instruments on the proposed 2009 Mars Science Lander (MSL) will be demonstrated. This instrument will be able to identify volatile compounds as well as resident organic molecules on the parts-per-billion (ppb) level. Also, it will be able to obtain an inventory of chemical species on the surface of Mars which will result in a better understanding of ongoing surface chemistry. Finally, questions relevant to biological processes will be answered with the complete inventory of surface and near surface organic molecules that the ESI/IMS/CIT is capable of performing.

  9. Development of a Linear Ion Trap Mass Spectrometer (LITMS) Investigation for Future Planetary Surface Missions

    Science.gov (United States)

    Brinckerhoff, W.; Danell, R.; Van Ameron, F.; Pinnick, V.; Li, X.; Arevalo, R.; Glavin, D.; Getty, S.; Mahaffy, P.; Chu, P.; Zacny, K.; Rogacki, S.; Grubisic, A.; Cornish, T.

    2014-01-01

    Future surface missions to Mars and other planetary bodies will benefit from continued advances in miniature sensor and sample handling technologies that enable high-performance chemical analyses of natural samples. Fine-scale (approx.1 mm and below) analyses of rock surfaces and interiors, such as exposed on a drill core, will permit (1) the detection of habitability markers including complex organics in association with their original depositional environment, and (2) the characterization of successive layers and gradients that can reveal the time-evolution of those environments. In particular, if broad-based and highly-sensitive mass spectrometry techniques could be brought to such scales, the resulting planetary science capability would be truly powerful. The Linear Ion Trap Mass Spectrometer (LITMS) investigation is designed to conduct fine-scale organic and inorganic analyses of short (approx.5-10 cm) rock cores such as could be acquired by a planetary lander or rover arm-based drill. LITMS combines both pyrolysis/gas chromatograph mass spectrometry (GCMS) of sub-sampled core fines, and laser desorption mass spectrometry (LDMS) of the intact core surface, using a common mass analyzer, enhanced from the design used in the Mars Organic Molecule Analyzer (MOMA) instrument on the 2018 ExoMars rover. LITMS additionally features developments based on the Sample Analysis at Mars (SAM) investigation on MSL and recent NASA-funded prototype efforts in laser mass spectrometry, pyrolysis, and precision subsampling. LITMS brings these combined capabilities to achieve its four measurement objectives: (1) Organics: Broad Survey Detect organic molecules over a wide range of molecular weight, volatility, electronegativity, concentration, and host mineralogy. (2) Organic: Molecular Structure Characterize internal molecular structure to identify individual compounds, and reveal functionalization and processing. (3) Inorganic Host Environment Assess the local chemical

  10. Microsystem with integrated capillary leak to mass spectrometer for high sensitivity temperature programmed desorption

    DEFF Research Database (Denmark)

    Quaade, Ulrich; Jensen, Søren; Hansen, Ole

    2004-01-01

    Temperature programmed desorption (TPD) is a method for obtaining information about quantities and binding properties of adsorbed species on a surface. A microfabricated flow system for TPD with an integrated capillary leak to a mass spectrometer is presented. The use of an integrated capillary l.......5 cm2 of platinum foil gives a clear desorption peak. By using the microfabricated flow system, TPD experiments can be performed in a carrier gas with a sensitivity approaching that of TPD experiments in vacuum. ©2004 American Institute of Physics...... leak minimizes dead volumes in the system, resulting in increased sensitivity and reduced response time. These properties make the system ideal for TPD experiments in a carrier gas. With CO desorbing from platinum as model system, it is shown that CO desorbing in 105 Pa of argon from as little as 0...

  11. A Low-Mass Drift Chamber System for the HADES-Spectrometer

    Science.gov (United States)

    Dohrmann, F.; Bethge, K.; Enghardt, W.; Fateev, O.; Garabatos, C.; Grosse, E.; Muentz, C.; Karig, W.; Koenig, W.; Smykov, L.; Sobiella, M.; Steigerwald, A.; Stelzer, H.; Stroth, J.; Wuestenfeld, J.; Zanewsky, Y.; Zentek, A.

    1998-11-01

    A new high resolution (Δ M/M < 1%) and high acceptance (45%) di-electron spectrometer (HADES) has been designed to investigate in-medium properties of hadrons. For tracking of all charged particles (in particular with sufficient resolution for electrons) a system of 24 low-mass drift chambers (Helium based counting gas and Aluminum field and cathode wires), arranged in four tracking planes, is used. Design aspects of the chambers are reported. Results of performance optimization using various prototype detectors are discussed, including results of an ageing test. Stable operation in the high-multiplicity environment of heavy ion collisions, and a spatial resolution of 70 μ m(σ) over 80% of a cell have been demonstrated in two beam experiments.

  12. Accelerator-mass spectrometer (AMS) radiocarbon dating of Pleistocene lake sediments in the Great Basin

    Science.gov (United States)

    Thompson, R.S.; Toolin, L.J.; Forester, R.M.; Spencer, R.J.

    1990-01-01

    Pleistocene lake sediments in the Great Basin typically contain little organic carbon, and thus are difficult to date reliably by conventional radioccarbon methods. Paleoenvironmental data are abundant in these sediments, but are of limited value without adequate age controls. With the advent of accelerator-mass spectrometer (AMS) radiocarbon dating, it is now possible to date these paleolacustrine sediments. AMS dates were obtained on sediment cores from the Bonneville, Franklin, and Lahontan Basins. In the Bonneville Basin, the AMS-based chronology compares well with other chronologies constructed from dated shore-zone features. In the Bonneville and Franklin basins, AMS dates delimit unconformities not apparent by other means. We found that dispersed organic carbon from sediments deposited during relatively freshwater intervals provided apparently reliable AMS radiocarbon dates. Carbonate microfossils from the Lahontan Basin also produced results that appear reasonable, while bulk carbonate yielded erroneous results. ?? 1990.

  13. Alternate technique for simultaneous measurement of photoionization cross-section of isotopes by TOF mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Saleem, M.; Amin, N.; Hussain, S.; Rafiq, M.; Mahmood, S.; Baig, M.A. [Quaid-i-Azam Univ., Dept. of Physics, Atomic and Molecular Physics Lab., Islamabad (Pakistan)

    2006-05-15

    New measurements of photoionization cross-sections of the lithium isotopes are reported employing a Time of Flight -TOF- mass spectrometer in conjunction with an atomic beam apparatus. Using a two-step selective photoionization and saturation technique, we have simultaneously measured the photoionization cross-section of the 2p excited state of both the isotopes Li{sup 6} and Li{sup 7} as 15 {+-} 2.5 Mb and 18 {+-} 2.5 Mb where the corresponding number densities have been determined as N{sub 0} {approx} 5.3*10{sup 10} atoms/cm{sup 3} and N{sub 0} {approx} 6.2*10{sup 11} atoms/cm{sup 3} respectively. (authors)

  14. Application of mass spectrometer-inverse gas chromatography to study polymer-solvent diffusivity and solubility.

    Science.gov (United States)

    Galdámez, J Román; Danner, Ronald P; Duda, J Larry

    2007-07-20

    The application of a mass spectrometer detector in capillary column inverse gas chromatography is shown to be a valuable tool in the measurement of diffusion and solubility in polymer-solvent systems. The component specific detector provides excellent results for binary polymer-solvent systems, but it is particularly valuable because it can be readily applied to multicomponent systems. Results for a number of infinitely dilute solvents in poly(vinyl acetate) (PVAc) are reported over a range of temperature from 60 to 150 degrees C. Results are also reported for finite concentrations of toluene and methanol in PVAc from 60 to 110 degrees C. Finally, the technique was applied to study the effect of finite concentrations of toluene on the diffusion coefficients of THF and cyclohexane in PVAc. The experimental data compare well with literature values for both infinite and finite concentrations, indicating that the experimental protocol described in this work is sound.

  15. Improving Mass Spectrometer Sensitivity Using a High-Pressure Electrodynamic Ion Funnel Interface

    Energy Technology Data Exchange (ETDEWEB)

    Ibrahim, Yehia M.; Tang, Keqi; Tolmachev, Aleksey V.; Shvartsburg, Alexandre A.; Smith, Richard D.

    2006-09-01

    We report on a new electrodynamic ion funnel that operates at a pressure of 30 Torr with no loss of ion transmission. The enhanced performance compared to previous ion funnel designs optimized for pressures of <5 Torr was achieved by reducing the ion funnel capacitance and increasing the RF drive frequency (1.7 MHz) and amplitude (100-170 V peak-to-peak). No degradation of ion transmission was observed for pressures from 2 - 30 Torr. The ability to operate at higher pressure enabled a new dual ion funnel mass spectrometer (MS) interface design that can accommodate a greater gas load. When combined with a multicapillary inlet, the interface provided more efficient introduction of ions, resulting in a significant enhancement in MS sensitivity and detection limits.

  16. Numerical investigation of ion transport in the interface region of mass spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Jugroot, M.; Groth, C.P.T. [Univ. of Toronto, Inst. for Aerospace Studies, Toronto, Ontario (Canada)]. E-mail: jugroot@utias.utoronto.ca; groth@utias.utoronto.ca; Thomson, B.A.; Baranov, V.; Collings, B.A. [MDS SCIEX, Concord, Ontario (Canada)

    2003-07-01

    The transport of free ions through highly under-expanded jet flows of neutral gases and in the presence of applied electric fields is investigated by continuum-based numerical simulations. A five-moment mathematical model and parallel multi-block numerical solution procedure is developed for predicting the ion transport. The model incorporates the effects of ion-neutral collision processes and is used in conjunction with a Navier-Stokes model and flow solver for the neutral gas to examine the key features of the ion motion. The influences of the neutral gas flow, electric field, and flow field geometry on ion mobility are all carefully assessed. Numerical results are given which are relevant to the ion flows occurring in the interface regions of mass spectrometer systems. (author)

  17. Numerical investigation of neutral flows in the interface region of mass spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Jugroot, M.; Groth, C.P.T. [Univ. of Toronto, Inst. for Aerospace Studies, Toronto, Ontario (Canada)]. E-mail: jugroot@utias.utoronto.ca; groth@utias.utoronto.ca; Thomson, B.A.; Baranov, V.; Collings, B.A. [MDS SCIEX, Concord, Ontario (Canada)]. E-mail: Bruce.Thomson@sciex.com; Vladimir.Baranov@sciex.com; Bruce.Collings@sciex.com

    2002-07-01

    The flow of neutral gas from atmospheric to near-vacuum conditions in the interface region of a mass-spectrometer is investigated by continuum-based numerical simulations. The key features of the neutral gas flow are examined and the influence of back pressure, orifice geometry, and gas skimmer configuration are assessed. The flow structure is shown to be that of a classical under-expanded free jet for 'skimmer-absent' cases and very good agreement between the numerical predictions and empirical and experimental values is demonstrated. For the 'skimmer-present' cases, the influence of the skimmer and the flow structure downstream of the orifice and skimmer are of particular interest and are investigated and discussed. (author)

  18. Multi-element and isotopic analyses of iron meteorites using a glow discharge mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Shimamura, Tadashi (Kitasato Univ., Sagamihara (Japan). School of Hygienic Sciences); Takahashi, Takako (Marubun Corp., Kotoku, Tokyo (Japan). Analytical Research Lab.); Honda, Masatake; Nagai, Hisao (Nihon Univ., Tokyo (Japan). Coll. of Humanities and Sciences)

    1993-04-01

    Multi-element and isotopic analyses were performed of eight iron meteorites using a glow discharge mass spectrometer. Virtually all the elements can be determined. Major components (Fe, Co and Ni) through to ultra-trace constituents at the sub ng g[sup -1] level (Sc etc.) are measured directly with minimum chemical treatment within the same analytical cycle. Extremely high relative concentrations of Ni, Cu, Pd, In, Sn, Sb, Te, Pb and Bi were found in the meteorite Yamato 791694; the concentration of C was also very high. The isotopic composition of Pb in this meteorite was close to primordial. Low concentrations of C, N and O were found in the meteorite Gibeon. Very low S and Zn and high Cr and V were found in a third meteorite, Chinga. An excess of [sup 53]Cr was observed in Yamato 75031, which was consistent with the cosmic ray production level expected from the concentration of [sup 45]Sc. (Author).

  19. The role of electron scattering from registration detector in the "Troitsk nu-mass" MAC-E type spectrometer

    Science.gov (United States)

    Grigorieva, P. V.; Nozik, A. A.; Pantuev, V. S.; Skasyrskaya, A. K.

    2016-10-01

    There is a proposal to search for a sterile neutrino in a few keV mass range by the "Troitsk nu-mass" facility. In order to estimate sterile neutrino mixing one needs to make precision spectrum measurements well below the endpoint using the existing electrostatic spectrometer with a magnetic adiabatic collimation, or MAC-E filter. The expected signature will be a kink in the electron energy spectrum in tritium beta-decay. In this paper we consider the systematic effect of electron backscattering on the detector used in the spectrometer. For this purpose we provide a set of Monte-Carlo simulation results of electron backscattering on a silicon detector with a thin golden window with realistic electric and magnetic fields in the spectrometer. We have found that the probability of such an effect reaches up to 20-30%. The scattered electron could be reflected backwards to the detector by electrostatic field or by magnetic mirror. There is also a few percent probability to escape from the spectrometer through its entrance. A time delay between the scattering on the detector and the return of the reflected electron can reach a couple of microseconds in the Troitsk spectrometer. Such estimations are critical for the planning upgrades of the detector and the registration electronics. All considered effects are relevant to any MAC-E type spectrometer with solid detector.

  20. Regiospecific analysis of neutral ether lipids by liquid chromatography/electrospray ionization/single quadrupole mass spectrometry: validation with synthetic compounds

    DEFF Research Database (Denmark)

    Hartvigsen, Karsten; Ravandi, A.; Bukhave, Klaus

    2001-01-01

    A reversed-phase high-performance liquid chromatography (HPLC) method with on-line electrospray ionization/collision-induced dissociation/mass spectrometry (ESI/CID/MS) is presented for the regiospecific analysis of synthetic reference compounds of neutral ether lipids. The reference compounds were...... characterized by chromatographic retention times, full mass spectra, and fragmentation patterns as an aid to clarify the regiospecificity of ether lipids from natural sources. The results clearly show that single quadrupole mass spectroscopic analysis may elucidate the regiospecific structure of neutral ether...... lipids. Ether lipid reference compounds were characterized by five to six major ions in the positive ion mode. The 1-O-alkyl-sn-glycerols were analyzed as the diacetoyl derivative, and showed the [M - acetoyl](+) ion as an important diagnostic ion. The diagnostic ions of directly analyzed 1-O- alkyl-2...

  1. Response of an aerosol mass spectrometer to organonitrates and organosulfates and implications for atmospheric chemistry.

    Science.gov (United States)

    Farmer, D K; Matsunaga, A; Docherty, K S; Surratt, J D; Seinfeld, J H; Ziemann, P J; Jimenez, J L

    2010-04-13

    Organonitrates (ON) are important products of gas-phase oxidation of volatile organic compounds in the troposphere; some models predict, and laboratory studies show, the formation of large, multifunctional ON with vapor pressures low enough to partition to the particle phase. Organosulfates (OS) have also been recently detected in secondary organic aerosol. Despite their potential importance, ON and OS remain a nearly unexplored aspect of atmospheric chemistry because few studies have quantified particulate ON or OS in ambient air. We report the response of a high-resolution time-of-flight aerosol mass spectrometer (AMS) to aerosol ON and OS standards and mixtures. We quantify the potentially substantial underestimation of organic aerosol O/C, commonly used as a metric for aging, and N/C. Most of the ON-nitrogen appears as NO(x)+ ions in the AMS, which are typically dominated by inorganic nitrate. Minor organonitrogen ions are observed although their identity and intensity vary between standards. We evaluate the potential for using NO(x)+ fragment ratios, organonitrogen ions, HNO(3)+ ions, the ammonium balance of the nominally inorganic ions, and comparison to ion-chromatography instruments to constrain the concentrations of ON for ambient datasets, and apply these techniques to a field study in Riverside, CA. OS manifests as separate organic and sulfate components in the AMS with minimal organosulfur fragments and little difference in fragmentation from inorganic sulfate. The low thermal stability of ON and OS likely causes similar detection difficulties for other aerosol mass spectrometers using vaporization and/or ionization techniques with similar or larger energy, which has likely led to an underappreciation of these species.

  2. Aerosol quantification with the Aerodyne Aerosol Mass Spectrometer: detection limits and ionizer background effects

    Directory of Open Access Journals (Sweden)

    F. Drewnick

    2008-10-01

    Full Text Available Systematic laboratory experiments were performed to investigate quantification of various species with two versions of the Aerodyne Aerosol Mass Spectrometer, a Q-AMS and a c-ToF-AMS. Here we present a new method to continuously determine the detection limits of the AMS analyzers during regular measurements, yielding DL information under various measurement conditions. Minimum detection limits range from 0.03 μg m−3 (nitrate, sulfate, and chloride up to 0.5 μg m−3 (organics for the Q-AMS. Those of the c-ToF-AMS are found between 0.003 μg m−3 (nitrate, sulfate and 0.03 μg m−3 (ammonium, organics. The DL values found for the c-ToF-AMS were ~10 times lower than those of the Q-AMS, mainly due to differences in ion duty cycle. Effects causing an increase of the detection limits include long-term instrument contamination, measurement of high aerosol mass concentrations and short-term instrument history. The self-cleaning processes which reduce the instrument background after measurement of large aerosol concentrations as well as the influences of increased instrument background on mass concentration measurements are discussed. Finally, improvement of detection limits by extension of averaging time intervals, selected or reduced ion monitoring, and variation of particle-to-background measurement ratio are investigated.

  3. Miniaturized Ion and Neutral Mass Spectrometer for CubeSat Atmospheric Measurements

    Science.gov (United States)

    Rodriguez, M.; Paschalidis, N.; Jones, S.; Sittler, E.; Chornay, D.; Uribe, P.; Cameron, T.

    2016-01-01

    To increase the number of single point in-situ measurements of thermosphere and exosphere ion and neutral composition and density, miniaturized instrumentation is in high demand to take advantage of the increasing platform opportunities available in the smallsat/cubesat industry. The INMS (Ion-Neutral Mass Spectrometer) addresses this need by providing simultaneous measurements of both the neutral and ion environment, essentially providing two instruments in one compact model. The 1.3U volume, 570 gram, 1.8W nominal power INMS instrument makes implementation into cubesat designs (3U and above) practical and feasible. With high dynamic range (0.1-500eV), mass dynamic range of 1-40amu, sharp time resolution (0.1s), and mass resolution of MdM16, the INMS instrument addresses the atmospheric science needs that otherwise would have required larger more expensive instrumentation. INMS-v1 (version 1) launched on Exocube (CalPoly 3U cubesat) in 2015 and INMS-v2 (version 2) is scheduled to launch on Dellingr (GSFC 6U cubesat) in 2017. New versions of INMS are currently being developed to increase and add measurement capabilities, while maintaining its smallsat/cubesat form.

  4. A high-resolution mass spectrometer to measure atmospheric ion composition

    Directory of Open Access Journals (Sweden)

    H. Junninen

    2010-02-01

    Full Text Available In this paper we present recent achievements on developing and testing a tool to detect the composition of ambient ions in the mass/charge range up to 2000 Th. The instrument is an Atmospheric Pressure Interface Time-of-Flight Mass Spectrometer (APi-TOF, Tofwerk AG. Its mass accuracy is better than 0.002%, and the mass resolving power is 3000 Th/Th. In the data analysis, a new efficient Matlab based set of programs (tofTools were developed, tested and used. The APi-TOF was tested both in laboratory conditions and applied to outdoor air sampling in Helsinki at the SMEAR III station. Transmission efficiency calibrations showed a throughput of 0.1–0.5% in the range 100–1300 Th for positive ions, and linearity over 3 orders of magnitude in concentration was determined. In the laboratory tests the APi-TOF detected sulphuric acid-ammonia clusters in high concentration from a nebulised sample illustrating the potential of the instrument in revealing the role of sulphuric acid clusters in atmospheric new particle formation. The APi-TOF features a high enough accuracy, resolution and sensitivity for the determination of the composition of atmospheric small ions although the total concentration of those ions is typically only 400–2000 cm-3. The atmospheric ions were identified based on their exact masses, utilizing Kendrick analysis and correlograms as well as narrowing down the potential candidates based on their proton affinities as well isotopic patterns. In Helsinki during day-time the main negative ambient small ions were inorganic acids and their clusters. The positive ions were more complex, the main compounds were (polyalkyl pyridines and – amines. The APi-TOF provides a near universal interface for atmospheric pressure sampling, and this key feature will be utilized in future laboratory and field studies.

  5. Fullerene Soot in Eastern China Air: Results from Soot Particle-Aerosol Mass Spectrometer

    Science.gov (United States)

    Wang, J.; Ge, X.; Chen, M.; Zhang, Q.; Yu, H.; Sun, Y.; Worsnop, D. R.; Collier, S.

    2015-12-01

    In this work, we present for the first time, the observation and quantification of fullerenes in ambient airborne particulate using an Aerodyne Soot Particle - Aerosol Mass Spectrometer (SP-AMS) deployed during 2015 winter in suburban Nanjing, a megacity in eastern China. The laser desorption and electron impact ionization techniques employed by the SP-AMS allow us to differentiate various fullerenes from other aerosol components. Mass spectrum of the identified fullerene soot is consisted by a series of high molecular weight carbon clusters (up to m/z of 2000 in this study), almost identical to the spectral features of commercially available fullerene soot, both with C70 and C60 clusters as the first and second most abundant species. This type of soot was observed throughout the entire study period, with an average mass loading of 0.18 μg/m3, accounting for 6.4% of the black carbon mass, 1.2% of the total organic mass. Temporal variation and diurnal pattern of fullerene soot are overall similar to those of black carbon, but are clearly different in some periods. Combining the positive matrix factorization, back-trajectory and analyses of the meteorological parameters, we identified the petrochemical industrial plants situating upwind from the sampling site, as the major source of fullerene soot. In this regard, our findings imply the ubiquitous presence of fullerene soot in ambient air of industry-influenced area, especially the oil and gas production regions. This study also offers new insights into the characterization of fullerenes from other environmental samples via the advanced SP-AMS technique.

  6. On Applicability of a Miniaturised Laser Ablation Time of Flight Mass Spectrometer for Trace Elements Measurements

    Directory of Open Access Journals (Sweden)

    Marek Tulej

    2012-01-01

    Full Text Available We present results from mass spectrometric analysis of NIST standard materials and meteoritic samples conducted by a miniaturised laser ablation mass spectrometer designed for space research. The mass analyser supports investigation with a mass resolution (/Δ ≈ 500–600 and dynamic range within seven decades. Nevertheless, to maintain an optimal spectral quality laser irradiances lower than ~1 GW/cm2 are applied so far which results in a spread of RSC values. To achieve the quantitative performance of mass analyser, various effects influencing RSC factors have to be investigated. In this paper we investigate influence of laser irradiance, sampling procedure and plasma chemistry on the quantitative elemental and isotopic analysis. The studies indicate necessity for accurate control of laser characteristics and acquisition procedure. A relatively low irradiance applied causes a negligible sample damage and allows for accumulation of large number of waveforms from one sample location. The procedure yields statistically well averaged data and allows a sensitive in-depth analysis. The quantitative analyses of isotopic composition can be performed with accuracy and precision better as 1% and 2%, for isotopic patterns of elements and clusters, respectively. The numerical integration methods would be preferred to achieve more accurate results. The measurements of Allende sample yield detection of Pb isotopic pattern, nevertheless cluster species are readily observed in spectrum and make the elemental analysis of other trace elements difficult due to isobaric interferences. These detections are of a considerable interest because of possible application of the instrument for in situ elemental and isotopic analysis and radiometric dating of solids.

  7. Compact Ion and Neutral Mass Spectrometer with Ion Drifts, Temperatures and Neutral Winds

    Science.gov (United States)

    Paschalidis, Nikolaos

    2016-07-01

    In situ measurements of atmospheric neutral and ion composition and density, temperatures, ion drifts and neutral winds, are in high demand to study the dynamics of the ionosphere-theremosphere-mesosphere system. This paper presents a compact Ion and Neutral Mass Spectrometer (INMS) with impended ion drifts and temperature, and neutral winds capability for in situ measurements of ions and neutrals H, He, N, O, N2, O2. The mass resolution M/dM is approximately 10 at an incoming energy range of 0-20eV. The goal is to resolve ion drifts in the range 0 to 3000m/sec with a resolution better than 50m/sec, and neutral winds in the range of 0 to 1000m/sec with similar resolution. For temperatures the goal is to cover a dynamic range of 0 to 5000K. The INMS is based on front end optics for ions and neutrals, pre acceleration, gated time of flight, top hat ESA, MCP detectors and compact electronics. The instrument is redundant for ions and neutrals with the ion and neutral sensor heads on opposite sides and with full electronics in the middle. The ion front end includes RPA for temperature scanning and neutral front end includes angular modulation and thermionic ionization and ion blocking grids. The electronics include fast electric gating, TOF electronics, TOF binning and C&DH digital electronics. The data package includes 400 mass bins each for ions and neutrals and key housekeeping data for instrument health and calibration. The data sampling can be commanded from 0.1 to 10 sec with 1sec nominal setting. The instrument has significant onboard storage capability and a data compression scheme. The mass spectrometer version of the instrument has been flown on the Exocube mission. The instrument occupied 1.5U volume, weighed only 560 g and required nominal power of 1.6W The ExoCube mission was designed to acquire global knowledge of in-situ densities of [H], [He], [O] and H+, He+, O+ in the upper ionosphere and lower exosphere in combination with incoherent scatter radar and

  8. Qualitative and quantitative determination of YiXinShu Tablet using ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry.

    Science.gov (United States)

    Sun, Zhi; Li, Zhuolun; Zuo, Lihua; Wang, Zhenhui; Zhou, Lin; Shi, Yingying; Kang, Jian; Zhu, Zhenfeng; Zhang, Xiaojian

    2017-08-24

    To clarify and quantify the chemical profile of YiXinShu Tablet rapidly, a feasible and accurate strategy was developed by applying ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry. A total of 105 components were identified, including 25 phenanthraquinones, 11 lactones, 19 lignans, 24 acids and 26 other compounds. Among them, 26 major compounds were unambiguously detected by comparing with reference standards. And 19 of these compounds in three batches of YiXinShu Tablet were selected for quantitative determination. (Z)-Ligustilide, salvianic acid A, salvianolic acid A, salvianolic acid B and rosmarinic acid were abundant in these three batches with contents over 1.000 mg/g. The established analysis methods were examined to be accurate and feasible. The results show that the ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry method has a powerful qualitative ability and promising quantitative application. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  9. Simultaneous determination of 3-monochloropropane-1,2-diol and acrylamide in food by gas chromatography-triple quadrupole mass spectrometry with coupled column separation.

    Science.gov (United States)

    Xu, Xiao-min; He, Hua-li; Zhu, Yan; Feng, Liang; Ying, Ying; Huang, Bai-fen; Shen, Hai-tao; Han, Jian-long; Ren, Yi-ping

    2013-01-14

    Both 3-monochloropropane-1,2-diol (3-MCPD) and acrylamide are contaminants found in heat-processed foods and their related products. A quantitative method was developed for the simultaneous determination of both contaminants in food by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The analytes were purified and extracted by the matrix solid-phase dispersion extraction (MSPDE) technique with Extrelut NT. A coupled column (a 3 m Innowax combined with a 30 m DB-5 ms) was developed to separate both compounds efficiently without derivatization. Triple quadrupole mass spectrometry in multiple reaction monitoring mode (MRM) was applied to suppress matrix interference and obtain good sensitivity in the determination of both analytes. The limit of detection (LOD) in the sample matrix was 5 μg kg(-1) for 3-MCPD or acrylamide. The average recoveries for 3-MCPD and acrylamide in different food matrices were 90.5-107% and 81.9-95.7%, respectively, with the intraday relative standard deviations (RSDs) of 5.6-13.5% and 5.3-13.4%, respectively. The interday RSDs were 6.1-12.6% for 3-MCPD and were 5.0-12.8% for acrylamide. Both contaminants were found in samples of bread, fried chips, fried instant noodles, soy sauce, and instant noodle flavoring. Neither 3-MCPD nor acrylamide was detected in the samples of dairy products (solid or liquid samples) and non-fried instant noodles. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Proton affinity determinations using the kinetic method in an ion trap mass spectrometer

    Science.gov (United States)

    Nourse, Bobette D.; Graham Cooks, R.

    1991-05-01

    Proton affinities for various compounds have been estimated using a quadrupole ion trap by generating and mass-selecting proton-bound dimers and measuring their dissociation kinetics (A-H+ -B --> AH+ + B and/or BH+ + A). From the relative abundances of the fragment ions ([BH+] and [AH+]), which are related to their relative proton affinities by ln ([AH+]/[BH+]) = [Delta]PA/RT, it is shown that the proton affinities of the alicyclic carboxylic acids decrease in the order: cyclohexane- > cyclopropane- > cyclopentane- > cyclobutanecarboxylic acid. Proton affinity values for these species, measured from their proton-bound dimers with specific ketones, esters and carboxylic acids of known PA, are determined to be 198.3 ± 0.2 kcal mol-1, 198.0 ± 0.2 kcal mol-1, 197.8 ± 0.2 kcal mol-1 and 197.0 ± 0.2 kcal mol-1, respectively. The major contribution to the estimated uncertainties in these values results from the uncertainties in literature proton affinity values for the reference compounds. Proton affinity differences of meta and para deuterated benzoic acid proton-bound to benzoic acid (kH/kD = 1.0 ± 0.1 and 0.9 ± 0.1, respectively), for acetophenone proton-bound to deuterated-acetophenone (C6H5C(O)CD3) (kH/kD = 0.7 ± 0.1) and for 2-pentanone proton-bound to deuterated 2-pentanone (CH3CH2CH2C(O)CH3) (kH/kD = 2.1 ± 0.2). These results, as well as those for the carboxylic acids and benzoic acids given above, are accounted for in terms of stabilizing electronic effects in the protonated molecules.

  11. Fragmentation reactions of labeled and untabeled Rhodamine B in a high-resolution Fourier transform ion cyclotron resonance mass spectrometer.

    Science.gov (United States)

    Clemen, Martin; Gernert, Claus; Peters, Jonathan; Grotemeyer, Jürgen

    2013-01-01

    The fragmentation reactions of Rhodamine B have been investigated by the use of electrospray ionization mass spectra in a high mass resolving ion cyclotron resonance mass spectrometer. Using high resolution, it could be shown that the loss of 44 mass units from the molecular ion is due to propane; the measured masses were inconsistent with loss of carbon dioxide. These conclusions are supported using deuterium-labeled Rhodamine B. This sample again only shows the loss of fully-deuterated propane verifying the high-resolution data. These findings illustrate very clearly that the conclusions based solely on low resolution spectra were false. The general implication on fragmentations of aromatic acids is discussed.

  12. Background due to stored electrons following nuclear decays in the KATRIN spectrometers and its impact on the neutrino mass sensitivity

    CERN Document Server

    Mertens, S; Fraenkle, F M; Furse, D; Glueck, F; Goerhardt, S; Hoetzel, M; Kaefer, W; Leiber, B; Thuemmler, T; Wandkowsky, N; Wolf, J

    2012-01-01

    The KATRIN experiment is designed to measure the absolute neutrino mass scale with a sensitivity of 200 meV at 90% C.L. by high resolution tritium beta-spectroscopy. A low background level of 10 mHz at the beta-decay endpoint is required in order to achieve the design sensitivity. In this paper we discuss a novel background source arising from magnetically trapped keV electrons in electrostatic retarding spectrometers. The main sources of these electrons are alpha-decays of the radon isotopes (219,220)Rn as well as beta-decays of tritium in the volume of the spectrometers. We characterize the expected background signal by extensive MC simulations and investigate the impact on the KATRIN neutrino mass sensitivity. From these results we refine design parameters for the spectrometer vacuum system and propose active background reduction methods to meet the stringent design limits for the overall background rate.

  13. Evolving mass spectra of the oxidized component of organic aerosol: results from aerosol mass spectrometer analyses of aged diesel emissions

    Directory of Open Access Journals (Sweden)

    A. M. Sage

    2007-07-01

    Full Text Available The species and chemistry responsible for secondary organic aerosol (SOA formation remain highly uncertain. Laboratory studies of the oxidation of individual, high-flux SOA precursors do not lead to particles with mass spectra (MS matching those of ambient aged organic material. And, the complexity of real organic particles challenges efforts to identify their chemical origins. We have previously hypothesized that SOA can form from the atmospheric oxidation of a large suite of precursors with varying vapor pressures. Here, we support this hypothesis by using an aerosol mass spectrometer to track the chemical evolution of diesel exhaust as it is photochemically oxidized in an environmental chamber. With explicit knowledge of the condensed-phase MS of the primary emissions from our engine, we are able to decompose each recorded MS into contributing primary and secondary spectra throughout the experiment. We find that the SOA MS becomes increasingly oxidized as a function of time, eventually reaching a final MS that closely resembles that of ambient aged organic particulate matter. This observation is consistent with the idea that lower vapor pressure, semi-volatile organic emissions can form condensable products with fewer generations of oxidation, and therefore, they form relatively less oxidized SOA very quickly.

  14. Development and characterization of a single particle laser ablation mass spectrometer (SPLAM for organic aerosol studies

    Directory of Open Access Journals (Sweden)

    F. Gaie-Levrel

    2011-07-01

    Full Text Available A single particle instrument has been developed for real-time analysis of organic aerosols. This instrument, named Single Particle Laser Ablation Mass Spectrometry (SPLAM, samples particles using an aerodynamic lens system for which the theoretical performances were calculated. At the outlet of this system, particle detection and sizing are realized using two continuous diode lasers operating at λ = 403 nm. Polystyrene Latex (PSL, sodium chloride (NaCl and dioctylphtalate (DOP particles were used to characterize and calibrate optical detection of SPLAM. The optical detection limit (DL and detection efficiency (DE were determined using size-selected DOP particles. The DE is ranging from 0.1 to 90 % for 100 and 350 nm DOP particles respectively and the SPLAM instrument is able to detect and size-resolve particles as small as 110–120 nm. Scattered light is detected by two photomultipliers and the detected signals are used to trigger a UV excimer laser (λ = 248 nm used for laser desorption ionization (LDI of individual aerosol particles. The formed ions are analyzed by a 1 m linear time-of-flight mass spectrometer in order to access to the chemical composition of individual particles. The TOF-MS detection limit for gaseous aromatic compounds was determined to be 0.85 attograms. DOP particles were also used to test the overall functioning of the instrument. The analysis of a secondary organic aerosol, formed in a smog chamber by the ozonolysis of indene, is presented as a first scientific application of the instrument. Single particle mass spectra are obtained with a global hit rate of 10 %. They are found to be very different from one particle to another, reflecting chemical differences of the analyzed particles, and most of the detected mass peaks are attributed to oxidized products of indene.

  15. Negative Electron Transfer Dissociation Sequencing of Increasingly Sulfated Glycosaminoglycan Oligosaccharides on an Orbitrap Mass Spectrometer

    Science.gov (United States)

    Leach, Franklin E.; Riley, Nicholas M.; Westphall, Michael S.; Coon, Joshua J.; Amster, I. Jonathan

    2017-09-01

    The structural characterization of sulfated glycosaminoglycan (GAG) carbohydrates remains an important target for analytical chemists attributable to challenges introduced by the natural complexity of these mixtures and the defined need for molecular-level details to elucidate biological structure-function relationships. Tandem mass spectrometry has proven to be the most powerful technique for this purpose. Previously, electron detachment dissociation (EDD), in comparison to other methods of ion activation, has been shown to provide the largest number of useful cleavages for de novo sequencing of GAG oligosaccharides, but such experiments are restricted to Fourier transform ion cyclotron resonance mass spectrometers (FTICR-MS). Negative electron transfer dissociation (NETD) provides similar fragmentation results, and can be achieved on any mass spectrometry platform that is designed to accommodate ion-ion reactions. Here, we examine for the first time the effectiveness of NETD-Orbitrap mass spectrometry for the structural analysis of GAG oligosaccharides. Compounds ranging in size from tetrasaccharides to decasaccharides were dissociated by NETD, producing both glycosidic and cross-ring cleavages that enabled the location of sulfate modifications. The highly-sulfated, heparin-like synthetic GAG, ArixtraTM, was also successfully sequenced by NETD. In comparison to other efforts to sequence GAG chains without fully ionized sulfate constituents, the occurrence of sulfate loss peaks is minimized by judicious precursor ion selection. The results compare quite favorably to prior results with electron detachment dissociation (EDD). Significantly, the duty cycle of the NETD experiment is sufficiently short to make it an effective tool for on-line separations, presenting a straightforward path for selective, high-throughput analysis of GAG mixtures. [Figure not available: see fulltext.

  16. First performance results of a mobile high-resolution MR-ToF mass spectrometer for in-situ analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lang, Johannes; Ebert, Jens [II. Physikalisches Institut, JLU Giessen (Germany); Dickel, Timo; Plass, Wolfgang; Geissel, Hans; Haettner, Emma; Scheidenberger, Christoph [II. Physikalisches Institut, JLU Giessen (Germany); GSI, Darmstadt (Germany); Yavor, Mikhail [RAS St. Petersburg (Russian Federation)

    2012-07-01

    A mobile multiple-reflection time-of-flight mass spectrometer (MR-TOF-MS) has been designed, built and commissioned. While other mobile mass spectrometers are restricted to low or medium mass resolving power, this MR-TOF-MS allows for the first time for a mass resolving power exceeding 100.000 and a sub ppm accuracy in a transportable format. It can thus resolve isobars and enables to accurately determine the composition and structure of biomolecules. An atmospheric pressure interface provides compatibility to various atmospheric ion sources. The mass spectrometer part comprises an RFQ mass filter, ion cooler, ion trap, time-of-flight analyzer and detector. Supply electronics, DAQ and control system are mounted together with the spectrometer into a single frame with a total volume of only 0.8 m{sup 3}. First results with the MR-TOF-MS are presented, and an overview of envisaged life science applications is given, such as realtime tissue recognition in electrosurgery, identification of mycotoxins and analysis of soil samples for environmental studies.

  17. Development of a Portable Single Photon Ionization-Photoelectron Ionization Time-of-Flight Mass Spectrometer

    Directory of Open Access Journals (Sweden)

    Yunguang Huang

    2015-01-01

    Full Text Available A vacuum ultraviolet lamp based single photon ionization- (SPI- photoelectron ionization (PEI portable reflecting time-of-flight mass spectrometer (TOFMS was designed for online monitoring gas samples. It has a dual mode ionization source: SPI for analyte with ionization energy (IE below 10.6 eV and PEI for IE higher than 10.6 eV. Two kinds of sampling inlets, a capillary inlet and a membrane inlet, are utilized for high concentration and trace volatile organic compounds, respectively. A mass resolution of 1100 at m/z 64 has been obtained with a total size of 40 × 31 × 29 cm, the weight is 27 kg, and the power consumption is only 70 W. A mixture of benzene, toluene, and xylene (BTX, SO2, and discharging products of SF6 were used to test its performance, and the result showed that the limit of quantitation for BTX is as low as 5 ppbv (S/N = 10 : 1 with linear dynamic ranges greater than four orders of magnitude. The portable TOFMS was also evaluated by analyzing volatile organic compounds from wine and decomposition products of SF6 inside of a gas-insulated switchgear.

  18. Performance report for the low energy compact radiocarbon accelerator mass spectrometer at Uppsala University

    Energy Technology Data Exchange (ETDEWEB)

    Salehpour, M., E-mail: mehran.salehpour@physics.uu.se [Department of Physics and Astronomy, Ion Physics, Applied Nuclear Physics Division, P.O. Box 516, SE-751 20 Uppsala (Sweden); Håkansson, K.; Possnert, G. [Department of Physics and Astronomy, Ion Physics, Applied Nuclear Physics Division, P.O. Box 516, SE-751 20 Uppsala (Sweden); Wacker, L.; Synal, H.-A. [Ion Physics, ETH Zurich, Otto-Stern-Weg 5, 8093 (Switzerland)

    2016-03-15

    A range of ion beam analysis activities are ongoing at Uppsala University, including Accelerator Mass Spectrometry (AMS). Various isotopes are used for AMS but the isotope with the widest variety of applications is radiocarbon. Up until recently, only the 5 MV Pelletron tandem accelerator had been used at our site for radiocarbon AMS, ordinarily using 12 MeV {sup 14,13,12}C{sup 3+} ions. Recently a new radiocarbon AMS system, the Green-MICADAS, developed at the ion physics group at ETH Zurich, was installed. The system has a number of outstanding features which will be described. The system operates at a terminal voltage of 175 kV and uses helium stripper gas, extracting singly charged carbon ions. The low- and high energy mass spectrometers in the system are stigmatic dipole permanent magnets (0.42 and 0.97 T) requiring no electrical power nor cooling water. The system measures both the {sup 14}C/{sup 12}C and the {sup 13}C/{sup 12}C ratios on-line. Performance of the system is presented for both standard mg samples as well as μg-sized samples.

  19. Performance report for the low energy compact radiocarbon accelerator mass spectrometer at Uppsala University

    Science.gov (United States)

    Salehpour, M.; Håkansson, K.; Possnert, G.; Wacker, L.; Synal, H.-A.

    2016-03-01

    A range of ion beam analysis activities are ongoing at Uppsala University, including Accelerator Mass Spectrometry (AMS). Various isotopes are used for AMS but the isotope with the widest variety of applications is radiocarbon. Up until recently, only the 5 MV Pelletron tandem accelerator had been used at our site for radiocarbon AMS, ordinarily using 12 MeV 14,13,12C3+ ions. Recently a new radiocarbon AMS system, the Green-MICADAS, developed at the ion physics group at ETH Zurich, was installed. The system has a number of outstanding features which will be described. The system operates at a terminal voltage of 175 kV and uses helium stripper gas, extracting singly charged carbon ions. The low- and high energy mass spectrometers in the system are stigmatic dipole permanent magnets (0.42 and 0.97 T) requiring no electrical power nor cooling water. The system measures both the 14C/12C and the 13C/12C ratios on-line. Performance of the system is presented for both standard mg samples as well as μg-sized samples.

  20. First Signal on the Cryogenic Fourier-Transform Ion Cyclotron Resonance Mass Spectrometer

    Science.gov (United States)

    Lin, Cheng; Mathur, Raman; Aizikov, Kostantin; O'Connor, Peter B.

    2009-01-01

    The construction and achievement of the first signal on a cryogenic Fourier-transform ion cyclotron resonance mass spectrometer (FT-ICR-MS) are reported here, demonstrating proof-of-concept of this new instrument design. Building the FTICR cell into the cold bore of a superconducting magnet provided advantages over conventional warm bore design. At 4.2 K, the vacuum system cryopumps itself, thus removing the requirement for a large bore to achieve the desired pumping speed for maintaining base pressure. Furthermore, because the bore diameter has been reduced, the amount of magnet wire needed to achieve high field and homogeneity was also reduced, greatly decreasing the cost/Tesla of the magnet. The current instrument implements an actively shielded 14-Tesla magnet of vertical design with an external matrix assisted laser desorption/ionization (MALDI) source. The first signal was obtained by detecting the laser desorbed/ionized (LDI) C60+• ions, with the magnet at 7 Tesla, unshimmed, and the preamplifier mounted outside of the vacuum chamber at room temperature. A subsequent experiment done with the magnet at 14 Tesla and properly shimmed produced a C60 spectrum showing ∼350,000 resolving power at m/z ∼720. Increased magnetic field strength improves many FTMS performance parameters simultaneously, particularly mass resolving power and accuracy. PMID:17931882

  1. Development of an Ion Mobility Spectrometry-Orbitrap Mass Spectrometer Platform

    Energy Technology Data Exchange (ETDEWEB)

    Ibrahim, Yehia M.; Garimella, Sandilya V. B.; Prost, Spencer A.; Wojcik, Roza; Norheim, Randolph V.; Baker, Erin S.; Rusyn, Ivan; Smith, Richard D.

    2016-12-20

    Complex samples benefit from multidimensional measurements where higher resolution enables more complete characterization of biological and environmental systems. To address this challenge, we developed a drift tube-based ion mobility spectrometry-Orbitrap mass spectrometer (IMS-Orbitrap MS) platform. To circumvent the time scale disparity between the fast IMS separation and the much slower Orbitrap MS acquisition, we utilized a dual gate and pseudorandom sequences to multiplexed injection of ions and allowing operation in signal averaging (SA), single multiplexing (SM) and double multiplexing (DM) IMS modes to optimize the signal-to-noise ratio of the measurements. For the SM measurements, a previously developed algorithm was used to reconstruct the IMS data. A new algorithm was developed for the DM analyses involving a two-step process that first recovers the SM data and then decodes the SM data. The algorithm also performs multiple refining procedures in order to minimize demultiplexing artifacts. The new IMS-Orbitrap MS platform was demonstrated by the analysis of proteomic and petroleum samples, where the integration of IMS and high mass resolution proved essential for accurate assignment of molecular formulae.

  2. Field testing of lake water chemistry with a portable and an AUV-based mass spectrometer.

    Science.gov (United States)

    Hemond, Harry F; Mueller, Amy V; Hemond, Michael

    2008-10-01

    Two mass spectrometers (MS) are tested for the measurement of volatile substances, such as hydrocarbons and metabolic gases, in natural waters. KOALA is a backpackable MS operated from above the water surface, in which samples are pumped through a flow cell using a syringe. NEREUS is an underwater instrument hosted by an autonomous underwater vehicle (AUV) that is linked to a communications network to provide chemical data in real time. The mass analyzers of the two MS are nearly identical cycloids, and both use flat-plate membrane inlets. Testing took place in an eutrophic, thermally stratified lake exhibiting steep chemical gradients and significant levels of methane. KOALA provided rapid multispecies analysis of dissolved gases, with a detection limit for methane of 0.1 ppm (readily extendable to 0.01 ppm) and savings of time of at least a factor of 10 compared to that of conventional analysis. The AUV-mounted NEREUS additionally provided rapid spatial coverage and the capability of performing chemical surveys autonomously. Tests demonstrated the need for temperature control of a membrane inlet when steep thermal gradients are present in a water body, as well as the benefits of co-locating all sensors on the AUV to avoid interference from chemically different waters entering and draining from the free-flooding outer hull. The ability to measure dissolved volatiles provided by MS offers potential for complementarity with ionic sensors in the study of natural waters, such as in the case of the carbonate system.

  3. Facility monitoring of toxic industrial compounds in air using an automated, fieldable, miniature mass spectrometer.

    Science.gov (United States)

    Smith, Jonell N; Keil, Adam; Likens, Jane; Noll, Robert J; Cooks, R Graham

    2010-05-01

    Gaseous samples of nine toxic industrial compounds (acrolein, acrylonitrile, carbon disulfide, cyanogen chloride, ethylene oxide, formaldehyde, hydrogen cyanide, phosgene, and sulfur dioxide) were detected, identified, and quantitated using a fully automated, fieldable, miniature mass spectrometer equipped with a glow discharge electron ionization source and a cylindrical ion trap mass analyzer. The instrument was outfitted with a combined direct air leak and dual thermal desorption tube inlet that allowed for continuous sampling of compounds with throughput times of 2 min or less. Most compounds showed a linear response over the concentration ranges studied (sub-parts per billion [ppb] to parts per million [ppm]). Sorbent tube limits of detection (20 ppb to 8 ppm for all analytes) were lower than those reported for the two compounds examined using direct leak (acrylonitrile 16 ppm and phosgene 500 ppb). All limits of detection were below the concentration at which the compound poses an immediate danger to life and health. Sensitivity, probability of true positives, and the false positive rate for each analyte were investigated and described using receiver operating characteristic (ROC) curves. High quality data with low false positive and negative rates are indicative of the good chemical specificity and sensitivity of the instrument. Complex matrices consisting of second-hand smoke, gasoline exhaust, diesel fuel exhaust, and multiple analytes were also studied. Detection limits for analytes generally increased in the mixtures, but analytes were still detected at concentrations as low as 100 ppb.

  4. Imaging and Rapid-Scanning Ion Mass Spectrometer (IRM) for the CASSIOPE e-POP Mission

    Science.gov (United States)

    Yau, Andrew W.; Howarth, Andrew; White, Andrew; Enno, Greg; Amerl, Peter

    2015-06-01

    The imaging and rapid-scanning ion mass spectrometer (IRM) is part of the Enhanced Polar Outflow Probe (e-POP) instrument suite on the Canadian CASSIOPE small satellite. Designed to measure the composition and detailed velocity distributions of ions in the ˜1-100 eV/q range on a non-spinning spacecraft, the IRM sensor consists of a planar entrance aperture, a pair of electrostatic deflectors, a time-of-flight (TOF) gate, a hemispherical electrostatic analyzer, and a micro-channel plate (MCP) detector. The TOF gate measures the transit time of each detected ion inside the sensor. The hemispherical analyzer disperses incident ions by their energy-per-charge and azimuth in the aperture plane onto the detector. The two electrostatic deflectors may be optionally programmed to step through a sequence of deflector voltages, to deflect ions of different incident elevation out of the aperture plane and energy-per-charge into the sensor aperture for sampling. The position and time of arrival of each detected ion at the detector are measured, to produce an image of 2-dimensional (2D), mass-resolved ion velocity distribution up to 100 times per second, or to construct a composite 3D velocity distribution by combining successive images in a deflector voltage sequence. The measured distributions are then used to investigate ion composition, density, drift velocity and temperature in polar ion outflows and related acceleration and transport processes in the topside ionosphere.

  5. Numerical investigation of interface region flows in mass spectrometers: ion transport

    Energy Technology Data Exchange (ETDEWEB)

    Jugroot, Manish [Institute for Aerospace Studies, University of Toronto, 4925 Dufferin Street, Toronto, Ontario, M3H 5T6 (Canada); Groth, Clinton P T [Institute for Aerospace Studies, University of Toronto, 4925 Dufferin Street, Toronto, Ontario, M3H 5T6 (Canada); Thomson, Bruce A [MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, L4K 4V8 (Canada); Baranov, Vladimir [MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, L4K 4V8 (Canada); Collings, Bruce A [MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, L4K 4V8 (Canada)

    2004-02-21

    The transport of free ions through highly under-expanded jet flows of neutral gases and in the presence of applied electric fields is investigated by continuum-based numerical simulations. In particular, numerical results are described that are relevant to ion flows occurring in the interface region of mass spectrometer systems. A five-moment mathematical model and parallel multi-block numerical solution procedure are developed for predicting the ion transport. The model incorporates the effects of ion-neutral collision processes and is used in conjunction with a Navier-Stokes model and flow solver for the neutral gas to examine the key features of the ion motion. The influences of the neutral gas flow, electric field, and flow field geometry on ion mobility are all carefully assessed. Several ions of varying mass and charge are considered, and the relative importance of competing effects (i.e. electric field and ion-neutral collision effects) is discussed. The capability of controlling the charged particle motions through a combination of directed neutral flow and applied electric field is demonstrated for high-speed, hypersonic jet flows.

  6. Characterization of ornidazole metabolites in human bile after intraveneous doses by ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    Jiangbo Du

    2012-04-01

    Full Text Available Ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS was used to characterize ornidazole metabolites in human bile after intravenous doses. A liquid chromatography tandem mass spectrometry (LC–MS/MS assay was developed for the determination of the bile level of ornidazole. Bile samples, collected from four patients with T-tube drainage after biliary tract surgery, were prepared by protein precipitation with acetonitrile before analysis. A total of 12 metabolites, including 10 novel metabolites, were detected and characterized. The metabolites of ornidazole in human bile were the products of hydrochloride (HCl elimination, oxidative dechlorination, hydroxylation, sulfation, diastereoisomeric glucuronation, and substitution of NO2 or Cl atom by cysteine or N-acetylcysteine, and oxidative dechlorination followed by further carboxylation. The bile levels of ornidazole at 12 h after multiple intravenous infusions were well above its minimal inhibitory concentration for common strains of anaerobic bacteria.

  7. Numerical modeling of flow in a differential chamber of the gas-dynamic interface of a portable mass-spectrometer

    Science.gov (United States)

    Pivovarova, E. A.; Smirnovsky, A. A.; Schmidt, A. A.

    2013-11-01

    Mathematical modeling of flow in the differential chamber of the gas-dynamic interface of a portable mass-spectrometer was carried out to comprehensively study the flow structure and make recommendations for the optimization of the gas-dynamic interface. Modeling was performed using an OpenFOAM open computational platform. Conditions for an optimal operating mode of the differential chamber were determined.

  8. Energy resolution methods efficiency depending on beam source position of potassium clusters in time-of-flight mass spectrometer

    Indian Academy of Sciences (India)

    Ş Şentürk; F Demiray; O Özsoy

    2007-09-01

    Energy resolution of the time-of-flight mass spectrometer was considered. The estimations indicate that the time-lag energy focusing method provides better resolution for the parallel case while the turnaround time is more convenient for the perpendicular position. Hence the applicability of the methods used for the energy resolution depends on beam source arrangement.

  9. The Varian MAT-250 mass spectrometer. Steady isotopes laboratory; Espectrometro de masas Varian MAT-250. Laboratorio de isotopos estables

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez M, V.; Tavera D, M.L. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, 11801 Mexico D.F. (Mexico)

    1997-07-01

    This work treats over the performance and applications of the Varian Mat-250 mass spectrometer which is in the environmental isotope laboratory. It can be applied over topics such as: ions formation, acceleration and collimation, ions separation, ions detection, data transformation, sampling, {delta} notation. (Author)

  10. Development and characterization of a single particle laser ablation mass spectrometer (SPLAM for organic aerosol studies

    Directory of Open Access Journals (Sweden)

    F. Gaie-Levrel

    2012-01-01

    Full Text Available A single particle instrument was developed for real-time analysis of organic aerosol. This instrument, named Single Particle Laser Ablation Mass Spectrometry (SPLAM, samples particles using an aerodynamic lens system for which the theoretical performances were calculated. At the outlet of this system, particle detection and sizing are realized by using two continuous diode lasers operating at λ = 403 nm. Polystyrene Latex (PSL, sodium chloride (NaCl and dioctylphtalate (DOP particles were used to characterize and calibrate optical detection of SPLAM. The optical detection limit (DL and detection efficiency (DE were determined using size-selected DOP particles. The DE ranges from 0.1 to 90% for 100 and 350 nm DOP particles respectively and the SPLAM instrument is able to detect and size-resolve particles as small as 110–120 nm. During optical detection, particle scattered light from the two diode lasers, is detected by two photomultipliers and the detected signals are used to trigger UV excimer laser (λ = 248 nm used for one-step laser desorption ionization (LDI of individual aerosol particles. The formed ions are analyzed by a 1 m linear time-of-flight mass spectrometer in order to access to the chemical composition of individual particles. The TOF-MS detection limit for gaseous aromatic compounds was determined to be 0.85 × 10−15 kg (∼4 × 103 molecules. DOP particles were also used to test the overall operation of the instrument. The analysis of a secondary organic aerosol, formed in a smog chamber by the ozonolysis of indene, is presented as a first application of the instrument. Single particle mass spectra were obtained with an effective hit rate of 8%. Some of these mass spectra were found to be very different from one particle to another possibly reflecting chemical differences within the investigated indene SOA particles. Our study shows that an exhaustive statistical analysis, over hundreds of particles

  11. STRAPS v1.0: evaluating a methodology for predicting electron impact ionisation mass spectra for the aerosol mass spectrometer

    Directory of Open Access Journals (Sweden)

    D. O. Topping

    2017-06-01

    Full Text Available Our ability to model the chemical and thermodynamic processes that lead to secondary organic aerosol (SOA formation is thought to be hampered by the complexity of the system. While there are fundamental models now available that can simulate the tens of thousands of reactions thought to take place, validation against experiments is highly challenging. Techniques capable of identifying individual molecules such as chromatography are generally only capable of quantifying a subset of the material present, making it unsuitable for a carbon budget analysis. Integrative analytical methods such as the Aerosol Mass Spectrometer (AMS are capable of quantifying all mass, but because of their inability to isolate individual molecules, comparisons have been limited to simple data products such as total organic mass and the O : C ratio. More detailed comparisons could be made if more of the mass spectral information could be used, but because a discrete inversion of AMS data is not possible, this activity requires a system of predicting mass spectra based on molecular composition. In this proof-of-concept study, the ability to train supervised methods to predict electron impact ionisation (EI mass spectra for the AMS is evaluated. Supervised Training Regression for the Arbitrary Prediction of Spectra (STRAPS is not built from first principles. A methodology is constructed whereby the presence of specific mass-to-charge ratio (m∕z channels is fitted as a function of molecular structure before the relative peak height for each channel is similarly fitted using a range of regression methods. The widely used AMS mass spectral database is used as a basis for this, using unit mass resolution spectra of laboratory standards. Key to the fitting process is choice of structural information, or molecular fingerprint. Our approach relies on using supervised methods to automatically optimise the relationship between spectral characteristics and these molecular

  12. STRAPS v1.0: evaluating a methodology for predicting electron impact ionisation mass spectra for the aerosol mass spectrometer

    Science.gov (United States)

    Topping, David O.; Allan, James; Rami Alfarra, M.; Aumont, Bernard

    2017-06-01

    Our ability to model the chemical and thermodynamic processes that lead to secondary organic aerosol (SOA) formation is thought to be hampered by the complexity of the system. While there are fundamental models now available that can simulate the tens of thousands of reactions thought to take place, validation against experiments is highly challenging. Techniques capable of identifying individual molecules such as chromatography are generally only capable of quantifying a subset of the material present, making it unsuitable for a carbon budget analysis. Integrative analytical methods such as the Aerosol Mass Spectrometer (AMS) are capable of quantifying all mass, but because of their inability to isolate individual molecules, comparisons have been limited to simple data products such as total organic mass and the O : C ratio. More detailed comparisons could be made if more of the mass spectral information could be used, but because a discrete inversion of AMS data is not possible, this activity requires a system of predicting mass spectra based on molecular composition. In this proof-of-concept study, the ability to train supervised methods to predict electron impact ionisation (EI) mass spectra for the AMS is evaluated. Supervised Training Regression for the Arbitrary Prediction of Spectra (STRAPS) is not built from first principles. A methodology is constructed whereby the presence of specific mass-to-charge ratio (m/z) channels is fitted as a function of molecular structure before the relative peak height for each channel is similarly fitted using a range of regression methods. The widely used AMS mass spectral database is used as a basis for this, using unit mass resolution spectra of laboratory standards. Key to the fitting process is choice of structural information, or molecular fingerprint. Our approach relies on using supervised methods to automatically optimise the relationship between spectral characteristics and these molecular fingerprints. Therefore

  13. Open Source Software Tool Skyline Reaches Key Agreement with Mass Spectrometer Vendors | Office of Cancer Clinical Proteomics Research

    Science.gov (United States)

    The full proteomics analysis of a small tumor sample (similar in mass to a few grains of rice) produces well over 500 megabytes of unprocessed "raw" data when analyzed on a mass spectrometer (MS). Thus, for every proteomics experiment there is a vast amount of raw data that must be analyzed and interrogated in order to extract biological information. Moreover, the raw data output from different MS vendors are generally in different formats inhibiting the ability of labs to productively work together.

  14. Accurate mass measurements for the confirmation of Sudan azo-dyes in hot chilli products by capillary liquid chromatography-electrospray tandem quadrupole orthogonal-acceleration time of flight mass spectrometry.

    Science.gov (United States)

    Calbiani, F; Careri, M; Elviri, L; Mangia, A; Zagnoni, I

    2004-11-26

    The potential of capillary liquid chromatography (microLC)-quadrupole/time-of-flight mass spectrometry (Q-TOF MS) for the confirmation of Sudan I, II, III and IV azo-dyes as contaminants in hot-chilli food products was demonstrated. Using the microLC-electrospray ionization (ESI)-Q-TOF MS technique, accurate mass measurements of Sudan dyes were performed both on standard solutions and on matrices. Precision of exact mass measurements was calculated taking into account the ion statistics according to the number of ion sampled in the measurement. Accurate mass measurements by MS/MS experiments were performed to elucidate azo-dye fragmentation patterns. Selectivity of the microLC-Q-TOF MS method was assessed by evaluating matrix suppression effects by pre-column injection of blank hot chilli tomato sauce matrices. The results were compared with those obtained on a LC-triple quadrupole-MS system. Confirmation of Sudan I present in hot chill tomato sauce samples was obtained by accurate mass measurements. In real samples trueness of exact mass measurements was estimated to be 1.6 and 4.4 ppm when calculated for hot chilli tomato sauce and hot chilli tomato with cheese sauce samples, respectively; precision was calculated around 9.5 ppm.

  15. A spectrometer for study of high mass objects created in relativistic heavy ion reactions

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, T.A.; Barish, K.N.; Batsouli, S.; Bennett, M.J.; Bennett, S.J.; Chikanian, A.; Coe, S.D.; Cormier, T.M.; Davies, R.R.; De Cataldo, G.; Dee, P.; Diebold, G.E.; Dover, C.B.; Ewell, L.A.; Emmet, W.; Fachini, P.; Fadem, B.; Finch, L.E.; George, N.K.; Giglietto, N.; Greene, S.V.; Haridas, P.; Hill, J.C. E-mail: jhill@iastate.edu; Hirsch, A.S.; Hoversten, R.A.; Huang, H.Z.; Jaradat, H.; Kim, B.; Kumar, B.S.; Lajoie, J.G.; Lainis, T.; Lewis, R.A.; Li, Q.; Li, Y.; Libby, B.; Majka, R.D.; Miller, T.E.; Munhoz, M.G.; Nagle, J.L.; Petridis, A.; Pless, I.A.; Pope, J.K.; Porile, N.T.; Pruneau, C.; Rabin, M.S.Z.; Reid, J.D.; Rimai, A.; Riso, J.; Rose, A.; Rotondo, F.S.; Sandweiss, J.; Scharenberg, R.P.; Skank, H.; Slaughter, A.J.; Sleage, G.; Smith, G.A.; Spinelli, P.; Srivastava, B.K.; Tincknell, M.L.; Toothacker, W.S.; Van Buren, G.; Wilson, W.K.; Wohn, F.K.; Wolin, E.J.; Xu, Z.; Zhao, K

    1999-11-21

    Experiment E864 at the Brookhaven AGS accelerator uses a high sensitivity, large acceptance spectrometer, designed to search for strangelets and other novel forms of matter produced in high-energy heavy ion collisions. The spectrometer has excellent acceptance and rate capabilities for measuring the production properties of known particles and nuclei such as p-bar, d-bar and {sup 6}He. The experiment uses a magnetic spectrometer and employs redundant time of flight and position detectors and a hadronic calorimeter. In this paper we describe the design and performance of the spectrometer.

  16. Development of a time-of-flight mass spectrometer for ion desorption studies at HiSOR

    CERN Document Server

    Fujii, K; Nakashima, Y; Waki, S; Sardar, S A; Yasui, Y; Wada, S I; Sekitani, T; Tanaka, K

    2001-01-01

    We have developed a time-of-flight mass spectrometer which is now under operation at HiSOR storage ring for research of photon stimulated ion desorption (PSID). The employment of the pulsed high voltage method as a trigger allowed us to perform the investigations at a multi bunch operation of the storage ring. The performance of this spectrometer was evaluated by applying to the PSID measurements of PMMA (poly-methylmethacrylate) thin films. The results are compared with those obtained at Photon Factory by using pulsed synchrotron radiation in a single bunch operation. The capabilities of the apparatus for ion desorption studies are discussed.

  17. Amine permeation sources characterized with acid neutralization and sensitivities of an amine mass spectrometer

    Science.gov (United States)

    Freshour, N. A.; Carlson, K. K.; Melka, Y. A.; Hinz, S.; Panta, B.; Hanson, D. R.

    2014-10-01

    An acid titration method for quantifying amine permeation rates was used to calibrate an Ambient pressure Proton transfer Mass Spectrometer (AmPMS) that monitors ambient amine compounds. The method involves capturing amines entrained in a N2 flow by bubbling it through an acidified solution (~10-5 M HCl), and the amines are quantified via changes in solution pH with time. Home-made permeation tubes had permeation rates (typically tens of pmol s-1) that depended on the type of amine and tubing and on temperature. Calibrations of AmPMS yielded sensitivities for ammonia, methylamine, dimethylamine, and trimethylamine that are close to the sensitivity assuming a gas-kinetic, ion-molecule rate coefficient. The permeation tubes were also designed to deliver a reproducible amount of amine to a flow reactor where nucleation with sulfuric acid was studied. The high proton affinity compound dimethyl sulfoxide (DMSO), linked to oceanic environments, was also studied and AmPMS is highly sensitive to it. AmPMS was deployed recently in two field campaigns and, using these sensitivities, mixing ratios for ammonia and the alkyl amines are derived from the signals. Correlations between these species and with particle formation events are discussed.

  18. Inductively coupled plasma mass spectrometer with laser ablation metal ions release detection in the human mouth

    Science.gov (United States)

    Kueerova, Hana; Dostalova, Tatjana; Prochazkova, J.

    2002-06-01

    Presence of more dental alloys in oral cavity often causes pathological symptoms. Due to various and multi-faced symptomatology, they tend to be a source of significant problems not only for the patient but also for the dentist. Metal ions released from alloys can cause subjective and objective symptoms in mouth. The aim of this study was detection of metal elements presence in saliva. There were 4 groups of examined persons: with intact teeth (15 individuals) with metallic restorations, pathological currents 5-30 (mu) A, multi-faced subjective symptomatology and uncharacteristic objective diagnosis (32 patients), with metallic restorations and no subjective symptoms (14 persons) and with metallic restorations, without pathological currents and with problems related to galvanism (13 patients). Presence of 14 metal elements was checked by inductively coupled plasma mass spectrometer with laser ablation. Nd:YAG laser detector was used. There were significant differences in content of silver, gold and mercury between persons with intact teeth and other three groups. There were no differences found between subjects with and without galvanic currents, and presence of subjective and objective symptoms.

  19. Mars Organic Molecule Analyzer (MOMA) mass spectrometer for ExoMars 2018 and beyond

    Science.gov (United States)

    Brinckerhoff, W. B.; Pinnick, V. T.; van Amerom, F. H. W.; Danell, R. M.; Arevalo, R. D.; Atanassova, M. S.; Li, Xiang; Mahaffy, P. R.; Cotter, R. J.; Goesmann, F.; Steininger, H.

    The 2018 joint ESA-Roscosmos ExoMars rover mission will seek the signs of past or present life in the near-surface environment of Mars. The rover will obtain samples from as deep as two meters beneath the surface and deliver them to an onboard analytical laboratory for detailed examination. The Mars Organic Molecule Analyzer (MOMA) investigation forms a core part of the sample analysis capability of ExoMars. Its top objective is to address the main “ life signs” goal of the mission through detailed chemical analysis of the acquired samples. MOMA characterizes organic compounds in the samples with a novel dual ion source ion trap mass spectrometer (ITMS). The ITMS supports both pyrolysis-gas chromatography (pyr-GC) and Mars ambient laser desorption/ionization (LDI) analyses in an extremely compact package. Combined with the unprecedented depth sampling capability of ExoMars, MOMA affords a broad and powerful search for organics over a range of preservational environments, volatility, and molecular weight.

  20. Effect of Vaporizer Temperature on Ambient Non-Refractory Submicron Aerosol Composition and Mass Spectra Measured by the Aerosol Mass Spectrometer

    Science.gov (United States)

    Aerodyne Aerosol Mass Spectrometers (AMS) are routinely operated with a constant vaporizer temperature (Tvap) of 600oC in order to facilitate quantitative detection of non-refractory submicron (NR-PM1) species. By analogy with other thermal desorption instrument...

  1. Demonstration of a VUV lamp photoionization source for improvedorganic speciation in an aerosol mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Northway, M.J.; Jayne, J.T.; Toohey, D.W.; Canagaratna, M.R.; Trimborn, A.; Akiyama, K-I.; Shimono, A.; Jimenez, J.L.; DeCarlo, P.F.; Wilson, K.R.; Worsnop, D.R.

    2007-10-03

    In recent years, the Aerodyne AerosolMass Spectrometer(AMS) has become a widely used tool for determining aerosol sizedistributions and chemical composition for non-refractory inorganic andorganic aerosol. The current version of the AMS uses a combination offlash thermal vaporization and 70 eV electron impact (EI) ionization.However, EI causes extensive fragmentation and mass spectra of organicaerosols are difficult to deconvolute because they are composites of theoverlapping fragmentation patterns of all species present. Previous AMSstudies have been limited to classifying organics in broad categoriessuch as oxidized and hydrocarbon-like." In this manuscript we present newefforts to gain more information about organic aerosol composition byemploying the softer technique of vacuum ultraviolet (VUV) ionization ina Time-of-Flight AMS (ToF-AMS). In our novel design a VUV lamp is placedin direct proximity of the ionization region of the AMS, with only awindow separating the lamp and the ionizer. This design allows foralternation of photoionization and electron impact ionization within thesame instrument on the timescale of minutes. Thus, the EI-basedquantification capability of the AMS is retained while improved spectralinterpretation is made possible by combined analysis of the complementaryVUV and EI ionization spectra. Photoionization and electron impactionization spectra are compared for a number of compounds including oleicacid, long chain hydrocarbons, and cigarette smoke. In general, the VUVspectra contain much less fragmentation than the EI spectra and for manycompounds the parent ion is the dominant ion in the VUV spectrum. As anexample of the usefulness of the integration of PI within the fullcapability of the ToF-AMS, size distributions and size-segregated massspectra are examined for the cigarette smoke analysis. As a finalevaluation of the new VUV module, spectra for oleic acid are compared tosimilar experiments conducted using the tunable VUV radiation

  2. Comprehensive metabolite profiling of Plantaginis Semen using ultra high performance liquid chromatography with electrospray ionization quadrupole time-of-flight tandem mass spectrometry coupled with elevated energy technique.

    Science.gov (United States)

    Wang, Dandan; Qi, Meng; Yang, Qiming; Tong, Renchao; Wang, Rui; Bligh, S W Annie; Yang, Li; Wang, Zhengtao

    2016-05-01

    Plantaginis Semen is commonly used in traditional medicine to treat edema, hypertension, and diabetes. The commercially available Plantaginis Semen in China mainly comes from three species. To clarify the chemical composition and distinct different species of Plantaginis Semen, we established a metabolite profiling method based on ultra high performance liquid chromatography with electrospray ionization quadrupole time-of-flight tandem mass spectrometry coupled with elevated energy technique. A total of 108 compounds, including phenylethanoid glycosides, flavonoids, guanidine derivatives, terpenoids, organic acids, and fatty acids, were identified from Plantago asiatica L., P. depressa Willd., and P. major L. Results showed significant differences in chemical components among the three species, particularly flavonoids. This study is the first to provide a comprehensive chemical profile of Plantaginis Semen, which could be involved into the quality control, medication guide, and developing new drug of Plantago seeds.

  3. Discrimination of leaves of Panax ginseng and P. quinquefolius by ultra high performance liquid chromatography quadrupole/time-of-flight mass spectrometry based metabolomics approach.

    Science.gov (United States)

    Mao, Qian; Bai, Min; Xu, Jin-Di; Kong, Ming; Zhu, Lin-Yin; Zhu, He; Wang, Qiang; Li, Song-Lin

    2014-08-01

    In present study, an ultra high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS/MS) based metabolomics approach was established to investigate the metabolic profiles and characteristic chemical markers for distinguishing between leaves of Panax ginseng (LPG) and Panax quinquefolius (LPQ). The UHPLC-QTOF-MS/MS data were subjected to principal component analysis (PCA) and orthogonal partial least squared discrimination analysis (OPLS-DA) to rapidly find the potential characteristic components of LPG and LPQ, and the identities of detected peaks including the potential characteristic components were elucidated. Totally, 86 components were identified from these 2 kinds of leaf samples, in which 9 ginsenosides could be regarded as the characteristic chemical markers for the discrimination of LPG from LPQ. These results suggested that UHPLC-QTOF-MS/MS based metabolomics approach is a powerful tool to rapidly find characteristic markers for the quality control of LPG.

  4. Ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry to identify contaminants in water: an insight on environmental forensics.

    Science.gov (United States)

    Masiá, Ana; Campo, Julian; Blasco, Cristina; Picó, Yolanda

    2014-06-06

    Ultra-high pressure liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QqTOF-MS) acquiring full scan MS data for quantification, and automatic data dependent information product ion spectra (IDA-MS/MS) without any predefinition of the ions by the user was checked for identifying organic contaminants in water samples. The use of a database with more than 2000 compounds achieved high confidence results for a wide number of contaminants based upon retention time, accurate mass, isotopic pattern and MS/MS library searching. More than 20 contaminants, mostly pharmaceuticals, but also mycotoxins and polyphenols were unambiguously identified. Furthermore, the combination of statistical data analysis using principal component analysis (PCA) followed by empirical formula calculation, on-line database searching and MS/MS fragment ion interpretation achieves not only the successful detection of unknown contaminants but also the selection of those relevant to different types of waters. Unknown compounds, such as C₂₀H₃₄O₃, were identified in waste water showing the prospects of this technique. A group of 42 currently used pesticides were selected as target compounds to evaluate the quantitative possibilities. Mean recoveries and percentage relative standard deviation (RSD) were 48-79% (4-20% RSD). The limit of detections ranged from 0.02 to 2 ng L(-1), with a validated limit of quantification of 2 ng L(-1) for water after solid-phase (SPE) isolation and concentration. The quantitative data obtained using UHPLC-QqTOF-MS were compared with those obtained using conventional LC-MS/MS with a triple quadrupole (QqQ).

  5. Qualitative and quantitative analysis on chemical constituents from Curculigo orchioides using ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    He, Yongjing; Dong, Xin; Jia, Xiaoxuan; Li, Mei; Yuan, Tingting; Xu, Hongtao; Qin, Luping; Han, Ting; Zhang, Qiaoyan

    2015-01-01

    A rapid ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC-ESI-Q-TOF/MS) method was developed for qualitative and quantitative determination of constituents in the rhizome of Curculigo orchioides. Qualitative analysis was performed on a Waters ACQUITY UHPLC @ HSS T3 column (1.8 μm 100 × 2.1mm) using gradient elution with mobile phase of 0.1% formic acid and acetonitrile. Quantitative analysis was performed on an Agilent ZORBAX Eclipse plus C18 column (1.7 μm 100 × 2.1mm) using gradient elution with mobile phase of 0.1% acetic acid and acetonitrile for at least 20 min. Quadrupole TOF/MS in either full scan mode or extracted ion mode was used for qualitative and quantitative analysis of the constituents. According to the mass spectrometric fragmentation mechanism and UHPLC-ESI-Q-TOF-MS data, chemical structures of 45 constituents in the rhizome of Curculigo orchioides, including 19 phenols and phenolic glycosides, 16 lignans and lignan glycosides, 8 triterpenoid saponins, one flavone and one sesquiterpene, were identified tentatively on-line without the time-consuming process of isolation. In addition, 8 phenolic glycosides including 5-hydroxymethylfurfural (HMF), 2-hydroxy-5-(2-hydroxyethyl) phenyl-β-D-glucopyranoside (HPG), anacardoside (ACD), orcinol glucoside (OGD), orcinol-1-O-β-D-apiofuranosyl-(1 → 6)-β-D-glucopyranoside (OAG), 2,6-dimethoxybenzoic acid (DBA), curculigoside (CUR) and curculigine A (CCL) were quantitated in 11 collected samples and 10 commercial samples from different providers. The results show that UHPLC-ESI-Q-TOF-MS is a viable method for analysis and quality evaluation of the constituents from the rhizome of Curculigo orchioides. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. [Application of gas chromatography-high resolution quadrupole time of flight mass spectrometry to the analysis of benzaldehyde, benzyl alcohol acetophenone and phenylacetaldehyde in complex aromatic samples].

    Science.gov (United States)

    Liu, Junyan; Cao, Zhe; Li, Jiwen; Wang, Zheming; Wang, Chuan; Gu, Songyuan

    2015-02-01

    The study focuses on the quantitative analytical characterization of benzaldehyde, benzyl alcohol, acetophenone and phenylacetaldehyde in complex aromatic samples by gas chromatography-high resolution quadrupole time of flight mass spectrometry (GC-QTOF MS). The four compounds in real sample were accurately qualified and quantified through a comprehensive analysis of the GC retention times and the accurate masses of the ion fragments obtained by the high resolution MS. The new method therefore effectively avoids the interference of the real sample substrate, which reduces the accuracy of the analysis results. The peak area of the characteristic ion fragment for each compound was used for quantitation calculation. The MS signal responses of the four compounds showed good linear relationships with the corresponding mass concentrations and the linear regression coefficients were greater than 0. 99. The method recoveries were 87. 97% - 103.01%. The limits of detection (LODs) were 0. 01, 0. 03, 0. 02 and 0. 01 mg/L for benzaldehyde, benzyl alcohol, acetophenone and phenylacetaldehyde respectively. The contents of the four compounds in three real samples were analyzed. The study provided a new strategy for oxygenate analysis in complex aromatic samples using GC-QTOF MS. By measuring the accurate masses, the new method reduces the reliance on chromatographic separation ability and makes up the shortcomings of the traditional GC-MS methods.

  7. Factor analysis of combined organic and inorganic aerosol mass spectra from high resolution aerosol mass spectrometer measurements

    Directory of Open Access Journals (Sweden)

    Y. L. Sun

    2012-05-01

    Full Text Available The high resolution mass spectra of organic and inorganic aerosols from aerosol mass spectrometer (AMS measurements were first combined into positive matrix factorization (PMF analysis to investigate the sources and evolution processes of atmospheric aerosols. The new approach is able to study the mixing of organic aerosols (OA and inorganic species, the acidity of OA factors, and the fragment ion patterns related to photochemical processing. In this study, PMF analysis of the unified AMS spectral matrices resolved 8 factors for the submicron aerosols measured at Queens College in New York City in summer 2009. The hydrocarbon-like OA (HOA and cooking OA (COA contain very minor inorganic species, indicating the different sources and mixing characteristics between primary OA and secondary species. The two factors that are primarily ammonium sulfate (SO4-OA and ammonium nitrate (NO3-OA, respectively, are overall neutralized, of which the OA in SO4-OA shows the highest oxidation state (O/C = 0.69 among OA factors. The semi-volatile oxygenated OA comprises two components, i.e., a less oxidized (LO-OOA and a more oxidized (MO-OOA. The MO-OOA represents a local photochemical product with the diurnal profile exhibiting a pronounced noon peak, consistent with those of formaldehyde (HCHO and Ox (= O3+NO2. The much higher NO+/NO2+ fragment ion ratio in MO-OOA than that from ammonium nitrate alone provides evidence for the formation of organic nitrates. The amine-related nitrogen-enriched OA (NOA contains ~25% of acidic inorganic salts, elucidating the formation of secondary OA from amines in acidic environments. The size distributions derived from 3-dimensional size-resolved mass spectra show distinct diurnal evolving behaviors for different OA factors, but overall a progressing evolution from smaller to larger particle mode as a function of oxidation states

  8. Toward a Fieldable Atomic Mass Spectrometer for Safeguards Applications: Sample Preparation and Ionization

    Energy Technology Data Exchange (ETDEWEB)

    Barinaga, Charles J.; Hager, George J.; Hart, Garret L.; Koppenaal, David W.; Marcus, R. Kenneth; Jones, Sarah MH; Manard, Benjamin T.

    2014-10-31

    The International Atomic Energy Agency’s (IAEA’s) long-term research and development plan calls for the development of new methods to detect misuse at nuclear fuel cycle facilities such as reprocessing and enrichment plants. At enrichment plants, for example, the IAEA’s contemporary safeguards approaches are based on a combination of routine and random inspections that include collection of UF6 samples from in-process material and selected cylinders for subsequent analyses. These analyses include destructive analysis (DA) in a laboratory (typically by mass spectrometry [MS]) for isotopic characterization, and environmental sampling (ES) for subsequent laboratory elemental and isotopic analysis (also both typically by MS). One area of new method development includes moving this kind of isotope ratio analytical capability for DA and ES activities into the field. Some of the reasons for these developments include timeliness of results, avoidance of hazardous material shipments, and guidance for additional sample collecting. However, this capability does not already exist for several reasons, such as that most lab-based chemical and instrumental methods rely on laboratory infrastructure (highly trained staff, power, space, hazardous material handling, etc.) and require significant amounts of consumables (power, compressed gases, etc.). In addition, there are no currently available, fieldable instruments for atomic or isotope ratio analysis. To address these issues, Pacific Northwest National Laboratory (PNNL) and collaborator, Clemson University, are studying key areas that limit the fieldability of isotope ratio mass spectrometry for atomic ions: sample preparation and ionization, and reducing the physical size of a fieldable mass spectrometer. PNNL is seeking simple and robust techniques that could be effectively used by inspectors who may have no expertise in analytical MS. In this report, we present and describe the preliminary findings for three candidate

  9. Application of MALDI-triple quadrupole mass spectrometry for the quantification of small molecules in biomedical research

    NARCIS (Netherlands)

    R.J.W. Meesters (Roland)

    2011-01-01

    textabstractA century after its introduction, mass spectrometry is still an innovative technology, which, due to continuous instrumental developments and improvements, has provided important scientific insights in biochemistry, molecular biology and medicine. Now, in 2011, mass spectrometry is used

  10. Application of MALDI-triple quadrupole mass spectrometry for the quantification of small molecules in biomedical research

    NARCIS (Netherlands)

    R.J.W. Meesters (Roland)

    2011-01-01

    textabstractA century after its introduction, mass spectrometry is still an innovative technology, which, due to continuous instrumental developments and improvements, has provided important scientific insights in biochemistry, molecular biology and medicine. Now, in 2011, mass spectrometry is used

  11. Comparison of two ionic liquid dispersive liquid-liquid microextraction approaches for the determination of benzoylurea insecticides in wastewater using liquid chromatography-quadrupole-linear ion trap-mass spectrometry: evaluation of green parameters.

    Science.gov (United States)

    Vázquez, M M Parrilla; Vázquez, P Parrilla; Galera, M Martínez; Moreno, A Uclés

    2014-08-22

    Two dispersive liquid-liquid microextraction (DLLME) approaches including temperature-controlled ionic liquid dispersive liquid-liquid microextraction (TCIL-DLLME) and ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (US-IL-DLLME) were compared for the extraction of six benzoylurea insecticides (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, lufenuron and flufenoxuron) from wastewater samples prior to their determination by high-performance liquid chromatography with a hybrid triple quadrupole-linear ion trap-mass spectrometer (LC-QqLIT-MS/MS). Influential parameters affecting extraction efficiency were systematically studied and optimized and the most significant green parameters were quantified and compared. The best results were obtained using the US-IL-DLLME procedure, which employed the IL 1-octyl-3-methylimidazolium hexafluorophosphate ([C8MIM][PF6]) and methanol (MeOH) as extraction and disperser solvent, respectively. US-IL-DLLME procedure was fast, easy, low environmental toxicity and, it was also able to successfully extract all selected benzoylureas. This method was extensively validated with satisfactory results: limits of detection and quantification were in the range 0.5-1.0 ng L(-1) and 1.5-3.5 ng L(-1), respectively, whereas recovery rates ranged from 89 to 103% and the relative standard deviations were lower than 13.4%. The applicability of the method was assessed with the analysis of effluent wastewater samples from a wastewater treatment plant located in an agricultural zone of Almería (Spain) and the results indicated the presence of teflubenzuron at mean concentration levels of 11.3 ng L(-1). US-IL-DLLME sample treatment in combination with LC-QqLIT-MS/MS has demonstrated to be a sensitive, selective and efficient method to determine benzoylurea insecticides in wastewaters at ultra-trace levels.

  12. Multidrug analysis of pharmaceutical and urine matrices by on-line coupled capillary electrophoresis and triple quadrupole mass spectrometry.

    Science.gov (United States)

    Maráková, Katarína; Piešt'anský, Juraj; Veizerová, Lucia; Galba, Jaroslav; Dokupilová, Svetlana; Havránek, Emil; Mikuš, Peter

    2013-06-01

    The present work illustrates potentialities of CE hyphenated with MS/MS for the simultaneous determination and identification of a mixture of simultaneously acting drugs in pharmaceutical and biological matrices. Here, the hyphenation was provided by ESI interface, while the MS/MS technique was based on the triple quadrupole configuration. Three drugs, namely pheniramine, phenylephrine, and paracetamol were determined and identified with high reliability due to their characterization in three different dimensions, i.e. electrophoresis and MS/MS, that prevented practically any interference. Appropriately selected transitions of the analytes (parent ion-quantifier product ion-qualifier product ion) provided their selective determination at maximum S/N. The proposed CE-MS/MS method was validated (LOD/LOQ, linearity, precision, recovery, accuracy) and applied for (i) the multidrug composition pharmaceuticals, namely Theraflu®, and (ii) human urine taken after per-oral administration of the same pharmaceutical preparation. The method was applied also for the investigation of potential weak associates of the drugs and monitoring of predicted (bio)degradation products of the drugs. Successful validation and application of the proposed method suggest its routine use in highly effective and reliable advanced drug control and biomedical research.

  13. A field-deployable, chemical ionization time-of-flight mass spectrometer: application to the measurement of gas-phase organic and inorganic acids

    Directory of Open Access Journals (Sweden)

    T. H. Bertram

    2011-03-01

    Full Text Available We report a new field-deployable chemical ionization time-of-flight mass spectrometer (CI-TOFMS for the direct measurement of trace gases in the atmosphere. We apply the technique to the measurement of gas-phase inorganic and organic acids via negative-ion proton transfer, using acetate as the reagent ion. A novel high pressure interface, incorporating two RF-only quadrupoles is used to efficiently focus ions through four stages of differential pumping before analysis with a compact TOFMS. The high ion-duty cycle (>20% of the TOFMS, coupled to efficient production and transmission of ions in the high pressure interface results in a highly sensitive (>300 ions s−1 pptv−1 instrument capable of the fast measurement of atmospheric gases at trace levels. We demonstrate the efficient transfer and detection of both bare ions and ion-molecule clusters, and characterize the instrument during field measurements aboard the R/V