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Sample records for quadrupole time-of-flight tandem

  1. [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.

  2. Rapid Identification of Steroidal Saponins in Trillium tschonoskii Maxim by Ultraperformance Liquid Chromatography Coupled to Electrospray Ionisation Quadrupole Time-of-Flight Tandem Mass Spectrometry.

    Science.gov (United States)

    Gao, Xin; Sun, Wenjun; Fu, Qiang; Niu, Xiaofeng

    2015-01-01

    Steroidal saponins in Trillium tschonoskii Maxim have many biological activities, including immunological regulation and anti-tumour. Comprehensive ingredient identification is critical for understanding its pharmacological mechanism and establishing quality control protocols. However, it is a challenging problem because of the complexity of steroidal saponins. To develop a UPLC-MS method for identifying and characterising steroidal saponins in the root and rhizome of T. tschonoskii. Methanolic extracts of T. tschonoskii were analysed by using ultraperformance liquid chromatography coupled to electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (UPLC-ESI/QTOF/MS). The UPLC experiments were performed by means of a reversed-phase C18 -column and a binary mobile phase system consisting of water and acetonitrile with formic acid under gradient elution conditions. For the UPLC-MS measurements, positive and negative ion modes were used in order to obtain better tandem mass spectra and high-resolution mass spectra. Based on retention times, accurate mass and mass spectrometric fragmentation, a total of 31 saponins distributed over eight steroidal aglycone skeletons were identified or tentatively elucidated from T. tschonoskii. The UPLC-ESI/QTOF/MS method has proven to be a powerful tool for rapid identification of steroidal saponins in T. tschonoskii without tedious and time-consuming isolation of pure constituents. Copyright © 2015 John Wiley & Sons, Ltd.

  3. Metabolism of Genipin in Rat and Identification of Metabolites by Using Ultraperformance Liquid Chromatography/Quadrupole Time-of-Flight Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Yue Ding

    2013-01-01

    Full Text Available The in vivo and in vitro metabolism of genipin was systematically investigated in the present study. Urine, plasma, feces, and bile were collected from rats after oral administration of genipin at a dose of 50 mg/kg body weight. A rapid and sensitive method using ultraperformance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-Q/TOF MS was developed for analysis of metabolic profile of genipin in rat biological samples (urine, plasma, feces, and bile. A total of ten metabolites were detected and identified by comparing their fragmentation patterns with that of genipin using MetaboLynx software tools. On the basis of the chromatographic peak area, the sulfated and glucuronidated conjugates of genipin were identified as major metabolites. And the existence of major metabolites G1 and G2 was confirmed by the in vitro enzymatic study further. Then, metabolite G1 was isolated from rat bile by semipreparative HPLC. Its structure was unambiguously identified as genipin-1-o-glucuronic acid by comparison of its UV, IR, ESI-MS, 1H-NMR, and 13C-NMR spectra with conference. In general, genipin was a very active compound that would transform immediately, and the parent form of genipin could not be observed in rats biological samples. The biotransformation pathways of genipin involved demethylated, ring-opened, cysteine-conjugated, hydroformylated, glucuronidated, and sulfated transformations.

  4. Metabolite characterization of a novel anti-cancer agent, icotinib, in humans through liquid chromatography/quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Liu, Dongyang; Jiang, Ji; Zhang, Li; Tan, Fenlai; Wang, Yingxiang; Hu, Pei

    2011-08-15

    Icotinib is a novel anti-cancer drug that has shown promising clinical efficacy and safety in patients with non-small-cell lung cancer (NSCLC). At this time, the metabolic fate of icotinib in humans is unknown. In the present study, a liquid chromatography/quadrupole time-of-flight tandem mass spectrometry (LC/Q-TOF MS) method was established to characterize metabolites of icotinib in human plasma, urine and feces. In addition, nuclear magnetic resonance (NMR) detection was utilized to determine the connection between side-chain and quinazoline groups for some complex metabolites. In total, 29 human metabolites (21 isomer metabolites) were characterized, of which 23 metabolites are novel compared to the metabolites in rats. This metabolic study revealed that icotinib was extensively metabolized at the 12-crown-4 ether moiety (ring-opening and further oxidation), carbon 15 (hydroxylation) and an acetylene moiety (oxidation) to yield 19 oxidized metabolites and to further form 10 conjugates with sulfate acid or glucuronic acid. To our knowledge, this is the first report of the human metabolic profile of icotinib. Study results indicated that significant attention should be paid to the metabolic profiles of NSCLC patients during the development of icotinib. Copyright © 2011 John Wiley & Sons, Ltd.

  5. Online extraction-high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry for rapid flavonoid profiling of Fructus aurantii immaturus.

    Science.gov (United States)

    Tong, Runna; Peng, Mijun; Tong, Chaoying; Guo, Keke; Shi, Shuyun

    2018-03-01

    Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC-DAD-QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction for Fructus aurantii immaturus (Zhishi), OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of eighteen flavonoids were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and compound 9, natsudaidain-3-O-glucoside, was discovered in Zhishi for the first time. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products. Copyright © 2018. Published by Elsevier B.V.

  6. Novel fluorinated surfactants tentatively identified in firefighters using liquid chromatography quadrupole time-of-flight tandem mass spectrometry and a case-control approach.

    Science.gov (United States)

    Rotander, Anna; Kärrman, Anna; Toms, Leisa-Maree L; Kay, Margaret; Mueller, Jochen F; Gómez Ramos, María José

    2015-02-17

    Fluorinated surfactant-based aqueous film-forming foams (AFFFs) are made up of per- and polyfluorinated alkyl substances (PFAS) and are used to extinguish fires involving highly flammable liquids. The use of perfluorooctanesulfonic acid (PFOS) and other perfluoroalkyl acids (PFAAs) in some AFFF formulations has been linked to substantial environmental contamination. Recent studies have identified a large number of novel and infrequently reported fluorinated surfactants in different AFFF formulations. In this study, a strategy based on a case-control approach using quadrupole time-of-flight tandem mass spectrometry (QTOF-MS/MS) and advanced statistical methods has been used to extract and identify known and unknown PFAS in human serum associated with AFFF-exposed firefighters. Two target sulfonic acids [PFOS and perfluorohexanesulfonic acid (PFHxS)], three non-target acids [perfluoropentanesulfonic acid (PFPeS), perfluoroheptanesulfonic acid (PFHpS), and perfluorononanesulfonic acid (PFNS)], and four unknown sulfonic acids (Cl-PFOS, ketone-PFOS, ether-PFHxS, and Cl-PFHxS) were exclusively or significantly more frequently detected at higher levels in firefighters compared to controls. The application of this strategy has allowed for identification of previously unreported fluorinated chemicals in a timely and cost-efficient way.

  7. Identification and characterization of vilazodone metabolites in rats and microsomes by ultrahigh-performance liquid chromatography/quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Chavan, Balasaheb B; Kalariya, Pradipbhai D; Tiwari, Shristy; Nimbalkar, Rakesh D; Garg, Prabha; Srinivas, R; Talluri, M V N Kumar

    2017-12-15

    Vilazodone is a selective serotonin reuptake inhibitor (SSRI) used for the treatment of major depressive disorder (MDD). An extensive literature search found few reports on the in vivo and in vitro metabolism of vilazodone. Therefore, we report a comprehensive in vivo and in vitro metabolic identification and structural characterization of vilazodone using ultrahigh-performance liquid chromatography/quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF/MS/MS) and in silico toxicity study of the metabolites. To identify in vivo metabolites of vilazodone, blood, urine and faeces samples were collected at different time intervals starting from 0 h to 48 h after oral administration of vilazodone to Sprague-Dawley rats. The in vitro metabolism study was conducted with human liver microsomes (HLM) and rat liver microsomes (RLM). The samples were prepared using an optimized sample preparation approach involving protein precipitation followed by solid-phase extraction. The metabolites have been identified and characterized by using LC/ESI-MS/MS. A total of 12 metabolites (M1-M12) were identified in in vivo and in vitro matrices and characterized by LC/ESI-MS/MS. The majority of the metabolites were observed in urine, while a few metabolites were present in faeces and plasma. Two metabolites were observed in the in vitro study. A semi-quantitative study based on percentage counts shows that metabolites M11, M6 and M8 were observed in higher amounts in urine, faeces and plasma, respectively. The structures of all the 12 metabolites were elucidated by using LC/ESI-MS/MS. The study suggests that vilazodone was metabolized via hydroxylation, dihydroxylation, glucuronidation, oxidative deamination, dealkylation, dehydrogenation and dioxidation. All the metabolites were screened for toxicity using an in silico tool. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Simultaneous determination of niacin and pyridoxine at trace levels by using diode array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Sel, Sabriye; Öztürk Er, Elif; Bakırdere, Sezgin

    2017-12-01

    A highly sensitive and simple diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method was developed for the simultaneous determination of niacin and pyridoxine in pharmaceutical drugs, tap water, and wastewater samples. To determine the in vivo behavior of niacin and pyridoxine, analytes were subjected to simulated gastric conditions. The calibration plots of the diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method showed good linearity over a wide concentration range with close to 1.0 correlation coefficients for both analytes. The limit of detection/limit of quantitation values for liquid chromatography quadrupole time-of-flight tandem mass spectrometry analysis were 1.98/6.59 and 1.3/4.4 μg/L for niacin and pyridoxine, respectively, while limit of detection/limit of quantitation values for niacin and pyridoxine in high-performance liquid chromatography analysis were 3.7/12.3 and 5.7/18.9 μg/L, respectively. Recovery studies were also performed to show the applicability of the developed methods, and percentage recovery values were found to be 90-105% in tap water and 94-97% in wastewater for both analytes. The method was also successfully applied for the qualitative and quantitative determination of niacin and pyridoxine in drug samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Analysis of 44 drugs of abuse and metabolites in wastewater and river water using a hybrid quadrupole time-of-flight tandem mass spectrometry

    Science.gov (United States)

    Andres-Costa, M. Jesus; Andreu, Vicente; Picó, Yolanda

    2016-04-01

    The presence of drugs of abuse in the aquatic environment has been recognized as an important issue for the ecosystem due their possible negative effect on it (Richardson, 2011). Incomplete removal of these substances during wastewater treatment could be one of the causes of their release in the environment (Zuccato and Castiglioni, 2009). Pollution by illicit drug residues at very low concentrations is generalized in populated areas, with potential risks for human health and the environment (Zuccato, 2008; Castiglioni et al 2007).The aim of this study was to screen and quantify 44 drugs of abuse and metabolites of wastewater samples using a hybrid quadrupole time-of-flight tandem mass spectrometry and furthermore carry out a post-target screening to identify additional compounds present in the water samples. Wastewater samples were collected from the influent and effluent of three wastewater treatment plants (WWTPs) in Valencia and river water samples form Turia River Basin. Illicit drugs were extracted by solid-phase extraction (SPE). The chromatography was performed with an Agilent 1260 Infinity ultra high performance liquid chromatography (UHPLC). The UHPLC system was coupled to a hybrid quadrupole time-of-flight ABSciex Triple TOFTM 5600. All analytes were analyzed in positive mode. Acquiring full scan MS data was employed for quantification of drugs of abuse, and automatic data dependent information product ion spectra (IDA-MS/MS) was checked for identifying emerging illicit drugs and other compounds in water samples. The use of a database containing 1212 compounds achieved high confidence results for a wide number of contaminants. In the present study, the presence of compounds that belong to amphetamines group (amphetamine, methamphetamine, ephedrine, MDMA, MDA and MDEA), tryptamines (bufotenine), pirrolidinophenone group (α-PVP and 4'-MePHP), arylcyclohexylamines (ketamine), cocainics (cocaine, benzoylecgonine, cocaethylene and ecgonine methyl ester) and

  10. 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...

  11. Implementation of dipolar direct current (DDC) collision-induced dissociation in storage and transmission modes on a quadrupole/time-of-flight tandem mass spectrometer.

    Science.gov (United States)

    Webb, Ian K; Londry, Frank A; McLuckey, Scott A

    2011-09-15

    Means for effecting dipolar direct current collision-induced dissociation (DDC CID) on a quadrupole/time-of-flight in a mass spectrometer have been implemented for the broadband dissociation of a wide range of analyte ions. The DDC fragmentation method in electrodynamic storage and transmission devices provides a means for inducing fragmentation of ions over a large mass-to-charge range simultaneously. It can be effected within an ion storage step in a quadrupole collision cell that is operated as a linear ion trap or as ions are continuously transmitted through the collision cell. A DDC potential is applied across one pair of rods in the quadrupole collision cell of a QqTOF hybrid mass spectrometer to effect fragmentation. In this study, ions derived from a small drug molecule, a model peptide, a small protein, and an oligonucleotide were subjected to the DDC CID method in either an ion trapping or an ion transmission mode (or both). Several key experimental parameters that affect DDC CID results, such as time, voltage, low mass cutoff, and bath gas pressure, are illustrated with protonated leucine enkephalin. The DDC CID dissociation method gives a readily tunable, broadband tool for probing the primary structures of a wide range of analyte ions. The method provides an alternative to the narrow resonance conditions of conventional ion trap CID and it can access more extensive sequential fragmentation, depending upon conditions. The DDC CID approach constitutes a collision analog to infrared multiphoton dissociation (IRMPD). Copyright © 2011 John Wiley & Sons, Ltd.

  12. Liquid chromatographic/electrospray ionization quadrupole/time of flight tandem mass spectrometric study of polyphenolic composition of different Vaccinium berry species and their comparative evaluation.

    Science.gov (United States)

    Ancillotti, Claudia; Ciofi, Lorenzo; Rossini, Daniele; Chiuminatto, Ugo; Stahl-Zeng, Jianru; Orlandini, Serena; Furlanetto, Sandra; Del Bubba, Massimo

    2017-02-01

    Ultra-high-performance liquid chromatography coupled with high-resolution quadrupole-time of flight mass spectrometry with both negative and positive ionization was used for comprehensively investigating the phenolic and polyphenolic compounds in berries from three spontaneous or cultivated Vaccinium species (i.e., Vaccinium myrtillus, Vaccinium uliginosum subsp. gaultherioides, and Vaccinium corymbosum). More than 200 analytes, among phenolic and polyphenolic compounds belonging to the classes of anthocyanins, monomeric and oligomeric flavonols, flavanols, dihydrochalcones, phenolic acids, together with other polyphenolic compounds of mixed structural characteristics, were identified. Some of the polyphenols herein investigated, such as anthocyanidin glucuronides and malvidin-feruloyl-hexosides in V. myrtillus, or anthocyanindin aldopentosides and coumaroyl-hexosides in V. uliginosum subsp. gaultherioides and a large number of proanthocyanidins with high molecular weight in all species, were described for the first time in these berries. Principal component analysis applied on original LC-TOF data, acquired in survey scan mode, successfully discriminated the three Vaccinium berry species investigated, on the basis of their polyphenolic composition, underlying one more time the fundamental role of mass spectrometry for food characterization.

  13. Characterization of the multiple components of Acanthopanax Senticosus stem by ultra high performance liquid chromatography with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Sun, Hui; Liu, Jianhua; Zhang, Aihua; Zhang, Ying; Meng, Xiangcai; Han, Ying; Zhang, Yingzhi; Wang, Xijun

    2016-02-01

    Acanthopanax Senticosus Harms. has been used widely in traditional Chinese medicine for the treatment of chronic bronchitis, neurasthenia, hypertension and ischemic heart disease. However, the in vivo constituents of the stem of Acanthopanax Senticosus remain unknown. In this paper, ultra high performance liquid chromatography with electrospray ionization quadrupole time-of-flight mass spectrometry and the MarkerLynx(TM) software combined with multiple data processing approach were used to study the constituents in vitro and in vivo. The aqueous extract from the Acanthopanax Senticosus stem and the compositions in rat serum after intragastric administration were completely analyzed. Consequently, 115 compounds in the aqueous extract from Acanthopanax Senticosus stem and 41 compounds absorbed into blood were characterized. Of the 115 compounds in vitro, 54 were reported for first time, including sinapyl alcohol, sinapyl alcohol diglucoside, and 1-O-sinapoyl-β-D-glucose. In the 41 compounds in vivo, 7 were prototype components and 34 were metabolites which were from 21 components of aqueous extract from Acanthopanax Senticosus stem, and the metabolic pathways of the metabolites were elucidated for first time. The results narrowed the range of screening the active components and provided a basis for the study of action mechanism and pharmacology. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Metabolic profiles of physalin A in rats using ultra-high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Feng, Xinchi; Liu, Hongxia; Chai, Liwei; Ding, Liqin; Pan, Guixiang; Qiu, Feng

    2017-03-01

    Physalin A, one of the major active components isolated from the calyces of Physalis alkekengi var. franchetii is considered to be a promising natural product due to its anti-inflammatory and excellent antitumor activities. Until now, only one paper is available from our group concerning identification of two sulfonate metabolites from rat feces after physalin A treatment. All the other researches related to physalin A were focused on its extraction, separation and biological activities. In this research, a rapid and reliable ultra-high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS/MS) method was developed and employed for the comprehensive study of the metabolism of physalin A in vivo for the first time. A total of 24 proposed metabolites were identified in plasma, bile, urine and feces of rats after oral administration of physalin A. The results indicated that sulfonation, reduction and hydroxylation were the major metabolic pathways of physalin A in vivo. Furthermore, this research provides scientific and reliable support for full understanding of the metabolism of physalin A and the results could help to elucidate the safety and efficacy of physalin A, as well as other physalins. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Systematic chemical profiling of Citrus grandis 'Tomentosa' by ultra-fast liquid chromatography/diode-array detector/quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Li, Pan-lin; Liu, Meng-hua; Hu, Jie-hui; Su, Wei-wei

    2014-03-01

    Citrus grandis 'Tomentosa', as the original plant of the traditional Chinese medicine "Huajuhong", has been used as antitussive and expectorant in clinic for thousands of years. The fruit epicarp and whole fruit of this plant were both literarily recorded and commonly used. In the present study, an ultra-fast liquid chromatography coupled with diode-array detection and quadrupole/time-of-flight mass spectrometry (UFLC-DAD-Q-TOF-MS/MS) based chemical profiling method was developed for rapid holistic quality evaluation of C. grandis 'Tomentosa', which laid basis for chemical comparison of two medicinal parts. As a result, forty-eight constituents, mainly belonging to flavonoids and coumarins, were unambiguously identified by comparison with reference standards and/or tentatively characterized by elucidating UV spectra, quasi-molecular ions and fragment ions referring to information available in literature. Both of the epicarp and whole fruit samples were rich in flavonoids and coumarins, but major flavonoids contents in whole fruit were significantly higher than in epicarp (P<0.5). The proposed method could be useful in quality control and standardization of C. grandis 'Tomentosa' raw materials and its products. Results obtained in this study will provide a basis for quality assessment and further study in vivo. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Urinary metabolomic profiling in rats exposed to dietary di(2-ethylhexyl) phthalate (DEHP) using ultra-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF-MS).

    Science.gov (United States)

    Dong, Xinwen; Zhang, Yunbo; Dong, Jin; Zhao, Yue; Guo, Jipeng; Wang, Zhanju; Liu, Mingqi; Na, Xiaolin; Wang, Cheng

    2017-07-01

    Di(2-ethylhexyl) phthalate (DEHP) is an omnipresent environmental chemical with widespread nonoccupational human exposure through multiple ways. Although considerable efforts have been invested to investigate mechanisms of DEHP toxicity, the key metabolic biomarkers of DEHP toxicity remain to be identified. The aim of this study was to assess the urinary metabonomics of dietary DEHP in rats using the technique of ultra-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF-MS). Fourteen female Wistar rats were divided into two groups and given increasing dietary doses of DEHP for 30 consecutive days. The urinary metabolite profile was studied using ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. Principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA) enabled clusters to be clearly separated. Eleven principal urinary metabolites were identified as contributing to the clusters. The clusters in the positive electrospray ionization (ESI) mode were xanthurenic acid, kynurenic acid, nonate, N6-methyladenosine, and L-isoleucyl-L-proline. The clusters in the negative ESI mode were hippuric acid, tetrahydrocortisol, citric acid, phenylpropionylglycine, cPA(18:2(9Z, 12Z)/0:0), and LysoPC(14:1(9Z)). The urinary metabonomic changes indicated that exposure to dietary DEHP can affect energy-related metabolism, liver and renal function, fatty acid metabolism, and cause DNA damage in rats. The findings of this study on the urinary metabolites and metabolic pathways of DEHP may form the basis for future studies on the mechanisms of toxicity of this commonly found environmental chemical.

  17. Determination of Grayanotoxins from Rhododendron brachycarpum in Dietary Supplements and Homemade Wine by Liquid Chromatography-Quadrupole Time-of-Flight-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Hwang, Taeik; Noh, Eunyoung; Jeong, Ji Hye; Park, Sung-Kwan; Shin, Dongwoo; Kang, Hoil

    2018-02-28

    A sensitive and specific high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry (LC-QTOF-MS) method combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of grayanotoxins I and III in dietary supplements and homemade wine. Grayanotoxins I and III were successfully extracted using solid-phase extraction cartridges, characterized by LC-QTOF-MS, and quantitated by LC-MS/MS. The LC-MS/MS calibration curves were linear over concentrations of 10-100 ng/mL (grayanotoxin I) and 20-400 ng/mL (grayanotoxin III). Grayanotoxins I and III were found in 51 foodstuffs, with quantitative determinations revealing total toxin concentrations of 18.4-101 000 ng/mL (grayanotoxin I) and 15.3-56 000 ng/mL (grayanotoxin III). The potential of the validated method was demonstrated by successful quantitative analysis of grayanotoxins I and III in dietary supplements and homemade wine; the method appears suitable for the routine detection of grayanotoxins I and III from Rhododendron brachycarpum.

  18. A metabolic way to investigate related hurdles causing poor bioavailability in oral delivery of isoacteoside in rats employing ultrahigh-performance liquid chromatography/quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Cui, Qingling; Pan, Yingni; Yan, Xiaowei; Qu, Bao; Liu, Xiaoqiu; Xiao, Wei

    2017-02-28

    Isoacteoside (ISAT), a phenylethanoid glycoside that acts as the principal bioactive component in traditional Chinese medicines, possesses broad pharmacological effects such as neuroprotective, antihypertensive and hepatoprotective activities. However, its pharmaceutical development has been severely limited due to the poor oral bioavailability. It is essential and significant to investigate related hurdles leading to the poor bioavailability of isoacteoside. Whole animal metabolism studies were conducted in rats, followed by metabolic mechanism including gastrointestinal stability, intestinal flora metabolism and intestinal enzyme metabolism employing the powerful method ultrahigh-performance liquid chromatography combined with quadrupole time-of-flight tandem mass spectrometry (UPLC/QTOF-MS/MS). A simple, rapid and sensitive method has been developed which comprehensively revealed the underlying cause of poor bioavailability of ISAT in a metabolic manner. The prototype of ISAT and its combined metabolites have not been detected in plasma. Furthermore, the residual content of the parent compound in in vitro experiments was approximately 59%, 5% and barely none in intestinal bacteria, intestinal S9 and simulated intestinal juice at 6 h, respectively. The present work has demonstrated that the factors causing the poor bioavailability of isoacteoside should be attributed to the metabolism. In general, the metabolism that resulted from intestinal flora and intestinal enzymes were predominant reasons giving rise to the poor bioavailability of ISAT, which also suggested that metabolites might be responsible for the excellent pharmacological effect of ISAT. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  19. Accurate determination of 3-alkyl-2-methoxypyrazines in wines by gas chromatography quadrupole time-of-flight tandem mass spectrometry following solid-phase extraction and dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Fontana, Ariel; Rodríguez, Isaac; Cela, Rafael

    2017-09-15

    A new reliable method for the determination 3-alkyl-2-methoxypyrazines (MPs) in wine samples based on the sequential combination of solid-phase extraction (SPE), dispersive liquid-liquid microextraction (DLLME) and gas chromatography (GC) quadrupole time-of-flight accurate tandem mass spectrometry (QTOF-MS/MS) is presented. Primary extraction of target analytes was carried out by using a reversed-phase Oasis HLB (200mg) SPE cartridge combined with acetonitrile as elution solvent. Afterwards, the SPE extract was submitted to DLLME concentration using 0.06mL carbon tetrachloride (CCl 4 ) as extractant. Under final working conditions, sample concentration factors above 379 times and limits of quantification (LOQs) between 0.3 and 2.1ngL -1 were achieved. Moreover, the overall extraction efficiency of the method was unaffected by the particular characteristics of each wine; thus, accurate results (relative recoveries from 84 to 108% for samples spiked at concentrations from 5 to 25ngL -1 ) were obtained using matrix-matched standards, without using standard additions over every sample. Highly selective chromatographic records were achieved considering a mass window of 5mDa, centered in the quantification product ion corresponding to each compound. Twelve commercial wines, elaborated with grapes from different varieties and geographical origins, were processed with the optimized method. The 2-isobutyl-3-methoxypyrazine (IBMP) was determined at levels above the LOQs of the method in half of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Application of characteristic ion filtering with ultra-high performance liquid chromatography quadrupole time of flight tandem mass spectrometry for rapid detection and identification of chemical profiling in Eucommia ulmoides Oliv.

    Science.gov (United States)

    He, Mingzhen; Jia, Jia; Li, Junmao; Wu, Bei; Huang, Wenping; Liu, Mi; Li, Yan; Yang, Shilin; Ouyang, Hui; Feng, Yulin

    2018-06-15

    Efficient targeted identification of chemical constituents from traditional Chinese medicine is still a major challenge. In this study, we used a characteristic ion filtering strategy to characterize compounds of Eucommia ulmoides Oliv. by ultra-high performance liquid chromatography quadrupole time of flight tandem mass spectrometry (UHPLC-ESI-Q-TOF-MS/MS). By using the ion filtering approach, target constituents of Eucommia ulmoides Oliv. were easily tentatively identified from the enormous LC/MS data set. The strategy consisted of the following three steps: 1) To establishing a characteristic ion database by diagnostic product ions or neutral loss fragments; 2) To evaluate the structural information of the compounds by high-resolution diagnostic characteristic ion filtering; 3) To confirm the different classes by chemical profiling according to their MS/MS spectra. In this study, characteristic ions are summarized as five major groups of compounds in Eucommia ulmoides Oliv. In total, 113 compounds were tentatively identified, including 23 potentially novel compounds. The results form a foundation for the quality control and chemical basis of Eucommia ulmoides Oliv. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Chemical Profiling of Re-Du-Ning Injection by Ultra-Performance Liquid Chromatography Coupled with Electrospray Ionization Tandem Quadrupole Time-of-Flight Mass Spectrometry through the Screening of Diagnostic Ions in MSE Mode

    Science.gov (United States)

    Wang, Zhenzhong; Geng, Jianliang; Dai, Yi; Xiao, Wei; Yao, Xinsheng

    2015-01-01

    The broad applications and mechanism explorations of traditional Chinese medicine prescriptions (TCMPs) require a clear understanding of TCMP chemical constituents. In the present study, we describe an efficient and universally applicable analytical approach based on ultra-performance liquid chromatography coupled to electrospray ionization tandem quadrupole time-of-flight mass spectrometry (UPLC-ESI-Q/TOF-MS) with the MSE (E denotes collision energy) data acquisition mode, which allowed the rapid separation and reliable determination of TCMP chemical constituents. By monitoring diagnostic ions in the high energy function of MSE, target peaks of analogous compounds in TCMPs could be rapidly screened and identified. “Re-Du-Ning” injection (RDN), a eutherapeutic traditional Chinese medicine injection (TCMI) that has been widely used to reduce fever caused by viral infections in clinical practice, was studied as an example. In total, 90 compounds, including five new iridoids and one new sesquiterpene, were identified or tentatively characterized by accurate mass measurements within 5 ppm error. This analysis was accompanied by MS fragmentation and reference standard comparison analyses. Furthermore, the herbal sources of these compounds were unambiguously confirmed by comparing the extracted ion chromatograms (EICs) of RDN and ingredient herbal extracts. Our work provides a certain foundation for further studies of RDN. Moreover, the analytical approach developed herein has proven to be generally applicable for profiling the chemical constituents in TCMPs and other complicated mixtures. PMID:25875968

  2. Metabolites identification of harmane in vitro/in vivo in rats by ultra-performance liquid chromatography combined with electrospray ionization quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Li, Shuping; Liu, Wei; Teng, Liang; Cheng, Xuemei; Wang, Zhengtao; Wang, Changhong

    2014-04-01

    Harmane, a β-carboline alkaloid with a wide spectrum of pharmacological activities, is naturally present in the human diet, in numerous foodstuffs and in hallucinogenic plants such as Peganum harmala, Banisteriopsis caapi and Tribulus terrestris. However, the precise metabolic fate of harmane remains unknown. In order to know whether harmane is extensively metabolized, a rapid and sensitive method using ultra-performance liquid chromatography combined with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC/ESI-QTOF-MS) was used to analyze the metabolic profile of harmane in vitro and in vivo in rats. A total of 21 metabolites were identified from the rat liver microsomes and rat liver S9 (9), rat urine (11), feces (16), bile (16), and plasma (10) after a single oral administration of harmane using MetaboLynx™ and MassFragment ™ software tools. It indicated that the biliary and faecal clearance were the major excretion routes for harmane as well as its metabolites. The specific CLogP values combined with different acidic and alkaline mobile phase were helpful and useful for distinguishing N-oxidation and monohydroxylation metabolites. The metabolic transformation pathways of harmane included monohydroxylation, dihydroxylation, N-oxidation, O-glucuronide conjugation, O-sulphate conjugation, and glutathione conjugation. In conclusion, this study showed an insight into the metabolism of harmane. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Metabolites profile of Gualou Xiebai Baijiu decoction (a classical traditional Chinese medicine prescription) in rats by ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Lin, Pei; Qin, Zifei; Yao, Zhihong; Wang, Li; Zhang, Weiyang; Yu, Yang; Dai, Yi; Zhou, Hua; Yao, Xinsheng

    2018-05-15

    Gualou Xiebai Baijiu decoction (GLXB), a well-known classic traditional Chinese medicine prescription, has been widely used to treat coronary heart diseases for thousands of years in Eastern Asian countries due to its remarkable clinical effect. However, due to lack of in vivo metabolism research, the chemical components responsible for the therapeutic effects still remain unclear. In this work, a reliable "representative structure based homologous xenobiotics identification" (RSBHXI) strategy based on ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF-MS) were applied to investigate the chemical components in GLXB extracts. As a result, 133 chemical components were characterized based on summarized fragmentation patterns, of which 41 components were confirmed unambiguously with authentic standards. Furthermore, a total of 138 GLXB-related xenobiotics were identified or tentatively characterized after oral administration of GLXB extracts. Moreover, to better understand the metabolic pathways of characteristic components in GLXB, metabolites profiles of five steroidal saponins and two flavonoids were performed, respectively. Since the metabolic pathways of five representative saponins had been finished in our previous study, we focused on the in vivo metabolism of two flavonoids. A total of 36 and 20 metabolites were detected in rat biological samples after oral administration of luteolin-7-O-β-D-glucopyranoside and rutin, respectively. The results indicated that dehydration, hydrolysis, hydroxylation, methylation, glucuronidation and sulfation were the main metabolic reactions, following the metabolic soft spots of GLXB-related flavonoids. Taken altogether, this study would be helpful for the further pharmacokinetics, pharmacological evaluation and quality control of GLXB. Copyright © 2018. Published by Elsevier B.V.

  4. Biotransformation and metabolic profile of Xian-Ling-Gu-Bao capsule, a traditional Chinese medicine prescription, with rat intestinal microflora by ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry analysis.

    Science.gov (United States)

    Gao, Meng-Xue; Tang, Xi-Yang; Zhang, Feng-Xiang; Yao, Zhi-Hong; Yao, Xin-Sheng; Dai, Yi

    2018-04-01

    Xian-Ling-Gu-Bao capsule (XLGB), a well-known traditional Chinese medicine prescription, has been used for the prevention and treatment of osteoporosis. The safety and efficacy of XLGB have been confirmed based on the principle of evidence-based medicine. XLGB is usually administered orally, after which its multiple components are brought into contact with intestinal microflora in the alimentary tract and biotransformed. However, investigations on the comprehensive metabolic profile of XLGB are absent. In this study, 12 representative compounds bearing different typical structures (including iridoid glycosides, prenylated flavonol glycosides, prenylated flavonoids, triterpenoid saponins, steroidal saponins, coumarins and monoterpene phenols) were selected and then investigated for their biotransformation in rat intestinal microflora. In addition, the metabolic profile of XLGB in rat intestinal microflora was investigated by ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. As a result, a total of 87 biotransformation components were identified from incubated solutions of 12 representative compounds and XLGB, which underwent 16 metabolic reactions (including deglycosylation, glycosylation, dehydrogenation, hydrogenation, oxidation, epoxidation, hydroxylation, dehydration, hydration, hydrolysis, methylation, isomerization, cyclization, pyrolysis reaction, amino acid conjugation and nucleophilic addition reaction with NH 3 ). This demonstrated that the deglycosylation reaction by cleavage of the sugar moieties is the main metabolic pathway of a variety of glycosides, including prenylated flavonol glycosides, coumarin glycosides, iridoid glycosides and saponins. In addition, compared with the biotransformation of 12 representative compounds, a different biotransformed fate was observed in the XLGB incubated samples of rat intestinal microflora. It is worth noting that the amino acid conjugation was first discovered

  5. Identification of regioisomers of methylated kaempferol and quercetin by ultra high performance liquid chromatography quadrupole time-of-flight (UHPLC–QTOF) tandem mass spectrometry combined with diagnostic fragmentation pattern analysis

    International Nuclear Information System (INIS)

    Ma, Chengying; Lv, Haipeng; Zhang, Xinzhong; Chen, Zongmao; Shi, Jiang; Lu, Meiling; Lin, Zhi

    2013-01-01

    Highlights: •Found methane elimination is position-specific for methylated flavonols. •Found retro Diels–Alder fragments retained methoxy at original ring of flavonols. •Proposed a diagnostic pattern for discriminating regioisomers of flavonols. •Identified the specificity of three novel flavonol O-methyltransferases. •Identified six biologically active compounds and four new compounds. -- Abstract: The O-methylation of active flavonoids can enhance their antiallergic, anticancerous, and cardioprotective effects depending on the methylation position. Thus, it is biologically and pharmacologically important to differentiate methylated flavonoid regioisomers. In this study, we examined the regioisomers of methylated kaempferol and quercetin using ultra high performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry. The methyl groups on the flavonoids can generally be cleaved as methyl radicals in a position-independent manner. We found that methyl groups can be cleaved as methane. If there are protons adjacent the methoxy on the flavonol rings, intra-molecule proton transfer can occur via collision-induced dissociation, and one molecule of methane can then be eliminated. The remaining charged fragment ([M+H−CH 4 ] + ) reflects the adjacent structure and is specific to the methoxy position. Furthermore, the retro Diels–Alder (RDA) fragmentation of methylated flavonols can generate fragments with the methoxy at the original methylated ring. Combining the position-specific [M+H−CH 4 ] + fragment with the RDA fragments provides a diagnostic pattern for rapidly identifying methylated regioisomeric flavonols. Along with their retention behaviour, we have successfully identified ten regioisomers of methylated kaempferol and quercetin, which include six compounds previously reported in plants and shown to be biologically active. The developed approach is sensitive, rapid, reliable, and requires few standard compounds. It is highly

  6. Sensitive characterization of polyphenolic antioxidants in Polygonatum odoratum by selective solid phase extraction and high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Hu, Xin; Zhao, Huading; Shi, Shuyun; Li, Hui; Zhou, Xiaoling; Jiao, Feipeng; Jiang, Xinyu; Peng, Dongming; Chen, Xiaoqin

    2015-08-10

    The complexity of natural products always leads to the co-elution of interfering compounds with bioactive compounds, which then has a detrimental effect on structural elucidation. Here, a new method, based on selective solid phase extraction combined with 1,1-diphenyl-2-picrylhydrazyl radical (DPPH) spiking and high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS), is described for sensitive screening, selective extraction and identification of polyphenolic antioxidants in Polygonatum odoratum. First, 25 polyphenolic antioxidants (1-25) were screened by DPPH spiking with HPLC. Second, polydopamine coated Fe3O4 microspheres (Fe3O4@PDA) were prepared to selectively extract target antioxidants with extraction efficiency from 55% to 100% when the amount of Fe3O4@PDA, extraction time, desorption solvent and time were 10mg, 20 min, acetonitrile, and 5 min. Third, 25 antioxidants (10 cinnamides and 15 homoisoflavanones) were identified by HPLC-DAD-QTOF-MS/MS. Furthermore, the DPPH scavenging activities of purified compounds (IC50, 1.6-32.8 μg/mL) validated the method. Among the identified antioxidants, four of them (12, 13, 18 and 19) were new compounds, four of them (2, 4, 8 and 14) were first obtained from family Liliaceae, five of them (1, 3, 5, 7 and 9) were first reported in genus Polygonatum, while one compound (24) was first identified in this species. The results indicated that the proposed method was an efficient and sensitive approach to explore polyphenolic antioxidants from complex natural products. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Proteomic analysis of proteins expressing in regions of rat brain by a combination of SDS-PAGE with nano-liquid chromatography-quadrupole-time of flight tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Maekawa Tsuyoshi

    2010-07-01

    Full Text Available Abstract Background Most biological functions controlled by the brain and their related disorders are closely associated with activation in specific regions of the brain. Neuroproteomics has been applied to the analysis of whole brain, and the general pattern of protein expression in all regions has been elucidated. However, the comprehensive proteome of each brain region remains unclear. Results In this study, we carried out comparative proteomics of six regions of the adult rat brain: thalamus, hippocampus, frontal cortex, parietal cortex, occipital cortex, and amygdala using semi-quantitative analysis by Mascot Score of the identified proteins. In order to identify efficiently the proteins that are present in the brain, the proteins were separated by a combination of SDS-PAGE on a C18 column-equipped nano-liquid chromatograph, and analyzed by quadrupole-time of flight-tandem-mass spectrometry. The proteomic data show 2,909 peptides in the rat brain, with more than 200 identified as region-abundant proteins by semi-quantitative analysis. The regions containing the identified proteins are membrane (20.0%, cytoplasm (19.5%, mitochondrion (17.1%, cytoskeleton (8.2%, nucleus (4.7%, extracellular region (3.3%, and other (18.0%. Of the identified proteins, the expressions of glial fibrillary acidic protein, GABA transporter 3, Septin 5, heat shock protein 90, synaptotagmin, heat shock protein 70, and pyruvate kinase were confirmed by immunoblotting. We examined the distributions in rat brain of GABA transporter 3, glial fibrillary acidic protein, and heat shock protein 70 by immunohistochemistry, and found that the proteins are localized around the regions observed by proteomic analysis and immunoblotting. IPA analysis indicates that pathways closely related to the biological functions of each region may be activated in rat brain. Conclusions These observations indicate that proteomics in each region of adult rat brain may provide a novel way to

  8. Identification of regioisomers of methylated kaempferol and quercetin by ultra high performance liquid chromatography quadrupole time-of-flight (UHPLC–QTOF) tandem mass spectrometry combined with diagnostic fragmentation pattern analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Chengying; Lv, Haipeng; Zhang, Xinzhong; Chen, Zongmao; Shi, Jiang [Tea Research Institute, Chinese Academy of Agricultural Sciences, 9 Meiling South Road, Hangzhou, Zhejiang 310008 (China); Lu, Meiling, E-mail: meilinglu@hotmail.com [Chemical Analysis Group, Agilent Technologies, No. 3 Wangjing North Road, Chaoyang Distr., Beijing 100102 (China); Lin, Zhi, E-mail: linz@mail.tricaas.com [Tea Research Institute, Chinese Academy of Agricultural Sciences, 9 Meiling South Road, Hangzhou, Zhejiang 310008 (China)

    2013-09-17

    Highlights: •Found methane elimination is position-specific for methylated flavonols. •Found retro Diels–Alder fragments retained methoxy at original ring of flavonols. •Proposed a diagnostic pattern for discriminating regioisomers of flavonols. •Identified the specificity of three novel flavonol O-methyltransferases. •Identified six biologically active compounds and four new compounds. -- Abstract: The O-methylation of active flavonoids can enhance their antiallergic, anticancerous, and cardioprotective effects depending on the methylation position. Thus, it is biologically and pharmacologically important to differentiate methylated flavonoid regioisomers. In this study, we examined the regioisomers of methylated kaempferol and quercetin using ultra high performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry. The methyl groups on the flavonoids can generally be cleaved as methyl radicals in a position-independent manner. We found that methyl groups can be cleaved as methane. If there are protons adjacent the methoxy on the flavonol rings, intra-molecule proton transfer can occur via collision-induced dissociation, and one molecule of methane can then be eliminated. The remaining charged fragment ([M+H−CH{sub 4}]{sup +}) reflects the adjacent structure and is specific to the methoxy position. Furthermore, the retro Diels–Alder (RDA) fragmentation of methylated flavonols can generate fragments with the methoxy at the original methylated ring. Combining the position-specific [M+H−CH{sub 4}]{sup +} fragment with the RDA fragments provides a diagnostic pattern for rapidly identifying methylated regioisomeric flavonols. Along with their retention behaviour, we have successfully identified ten regioisomers of methylated kaempferol and quercetin, which include six compounds previously reported in plants and shown to be biologically active. The developed approach is sensitive, rapid, reliable, and requires few standard

  9. Study on transfer rule of chemical constituents of tianshu capsule in productive process by high-performance liquid chromatography coupled with diode-array detection and quadrupole time-of-flight tandem mass spectrometry

    International Nuclear Information System (INIS)

    Lian, Y.P.; Xie, D.W.; Li, Y.J.; Xiao, W.; Huang, W.Z.; Ding, G.

    2016-01-01

    To develop a sensitive and accurate method for the fingerprint study and transfer rule of chemical constituents from Ligusticum chuanxiong Hort and Gastrodia elata Blume to Tianshu capsule in productive process, a high performance liquid chromatography coupled with diode-array detection and electrospray ionization quadrupole time-of-flight mass spectrometry (LC/QTOF-MS) method was established for analysis. The reference fingerprints of aqueous extract intermediate of medicinal material, alcohol extract intermediate of medicinal material and Tianshu capsule was established. The methodology was studied and the similarity was more than 0.99. The chromatographic methods demonstrated a good precision, repeatability, stability, with relative standard deviations of less than 3 percent for relative retention time and relative peak area. According to these fingerprints, some chemical constituents in the fingerprints were identified or tentatively identified based on their retention time, exact molecular weight and literature. Among of them 26 constituents were from Ligusticum chuanxiong Hort and nine components were from Gastrodia elata Blume. 25 out of 26 compounds had entered a transfer process and 17 compounds were transferred from intermediates to the final preparation, the Tianshu capsule. Thus, it is reasonable enough to use this transfer process to demonstrate the production technology. To sum up, this method is sensitive, accurate and useful,and it could provide us an approach to evaluate the production technology of Tianshu capsule. (author)

  10. Rapid Quadrupole-Time-of-Flight Mass Spectrometry Method Quantifies Oxygen-Rich Lignin Compound in Complex Mixtures

    Science.gov (United States)

    Boes, Kelsey S.; Roberts, Michael S.; Vinueza, Nelson R.

    2018-03-01

    Complex mixture analysis is a costly and time-consuming task facing researchers with foci as varied as food science and fuel analysis. When faced with the task of quantifying oxygen-rich bio-oil molecules in a complex diesel mixture, we asked whether complex mixtures could be qualitatively and quantitatively analyzed on a single mass spectrometer with mid-range resolving power without the use of lengthy separations. To answer this question, we developed and evaluated a quantitation method that eliminated chromatography steps and expanded the use of quadrupole-time-of-flight mass spectrometry from primarily qualitative to quantitative as well. To account for mixture complexity, the method employed an ionization dopant, targeted tandem mass spectrometry, and an internal standard. This combination of three techniques achieved reliable quantitation of oxygen-rich eugenol in diesel from 300 to 2500 ng/mL with sufficient linearity (R2 = 0.97 ± 0.01) and excellent accuracy (percent error = 0% ± 5). To understand the limitations of the method, it was compared to quantitation attained on a triple quadrupole mass spectrometer, the gold standard for quantitation. The triple quadrupole quantified eugenol from 50 to 2500 ng/mL with stronger linearity (R2 = 0.996 ± 0.003) than the quadrupole-time-of-flight and comparable accuracy (percent error = 4% ± 5). This demonstrates that a quadrupole-time-of-flight can be used for not only qualitative analysis but also targeted quantitation of oxygen-rich lignin molecules in complex mixtures without extensive sample preparation. The rapid and cost-effective method presented here offers new possibilities for bio-oil research, including: (1) allowing for bio-oil studies that demand repetitive analysis as process parameters are changed and (2) making this research accessible to more laboratories. [Figure not available: see fulltext.

  11. 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...... the absolute quantification of hundreds of molecular glycerophospholipid species, glycerolipid species, sphingolipid species and sterol lipids. Future applications in clinical cohort studies demand detailed lipid molecule information and the application of high-throughput lipidomics platforms. In this review...... we describe a novel high-throughput shotgun lipidomic platform based on 96-well robot-assisted lipid extraction, automated sample infusion by mircofluidic-based nanoelectrospray ionization, and quantitative multiple precursor ion scanning analysis on a quadrupole time-of-flight mass spectrometer...

  12. Analysis of phosphatidylcholine oxidation products in human plasma using quadrupole time-of flight mass spectrometry

    OpenAIRE

    Adachi, Junko; Asano, Migiwa; Yoshioka, Naoki; Nushida, Hideyuki; Ueno, Yasuhiro

    2006-01-01

    We report here an application of the previous method for the analysis ofphosphatidylcholine (PC) and lysophosphatidylcholine (lysoPC) oxidation products inhuman plasma using quadrupole time of flight (Q-TOF) mass spectrometry withelectrospray ionization. We separated these products using an HPLC C8 column witha gradient of methanol and 10 mM aqueous ammonium acetate. Monohydroperoxides,epoxyhydroxy derivatives, oxo derivatives, and trihydroxides of palmitoyl-linoleoyl(C16:0/C18:2) PC and stea...

  13. Application of a highly sensitive magnetic solid phase extraction for phytochemical compounds in medicinal plant and biological fluids by ultra-high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Cao, Wan; Yi, Ling; Ye, Li-Hong; Cao, Jun; Hu, Shuai-Shuai; Xu, Jing-Jing; Peng, Li-Qing; Zhu, Qiong-Yao; Zhang, Qian-Yun

    2015-10-01

    A highly sensitive method using reduced graphene oxide with iron oxide (rGO/Fe3 O4 ) as the sorbent in magnetic SPE has been developed for the purification of five anthraquinones (emodin, rhein, aloeemodin, physcion, and chrysophanol) in rhubarb and rat urine by ultra-HPLC coupled with quadrupole TOF/MS. The extraction was accomplished by adding trace amount rGO/Fe3 O4 suspension to 200 mL of aqueous mixture, and the excellent adsorption capacity of the nanoparticles was fully demonstrated in this procedure. Under the optimized conditions, the calibration curves were linear in the concentration range of 0.05-27.77 ng/mL with correlation coefficients varying from 0.9902 to 0.9978. The LODs ranged from 0.28 to 58.99 pg/mL. The experimental results indicated that the proposed method was feasible for the analysis of anthraquinones in rhubarb and urine samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  15. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  16. Neutral particle time-of-flight analyzer for the Tandem Mirror Experiment Upgrade (TMX-U)

    International Nuclear Information System (INIS)

    Hibbs, S.M.; Carter, M.R.; Coutts, G.W.

    1985-01-01

    We describe the design and performance of a time-of-flight (ToF) analyzer being built for installation on the east end cell of the Tandem Mirror Experiment Upgrade (TMX-U). Its primary purpose is to measure the velocity distribution of escaping charge exchange neutral particles having energies between 20 and 5000 electron volts (eV). It also enables direct determination of the thermal barrier potential when used in conjunction with the plasma potential diagnostic and the end loss ion spectrometer. In addition, it can measure the velocity distribution of passing ions leaving the central cell and of ions trapped in the thermal barrier

  17. Structural elucidation and identification of a new derivative of phenethylamine using quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Sekuła, Karolina; Zuba, Dariusz

    2013-09-30

    In recent years, the phenomenon of uncontrolled distribution of new psychoactive substances that were marketed without prior toxicological studies has been observed. Because many designer drugs are related in chemical structure, the potential for misidentifying them is an important problem. It is therefore essential to develop an analytical procedure for unequivocal elucidation of the structures of these compounds. The issue has been discussed in the context of 25I-NBMD [2-(4-iodo-2,5-dimethoxyphenyl)-N-[(2,3-methylenedioxyphenyl)methyl]ethanamine], a psychoactive substance first discovered on the drug market in 2012. The substance was extracted from blotter papers with methanol. Separation was achieved via liquid chromatography. Analysis was conducted by electrospray ionization quadrupole time-of-flight mass spectrometry (ESI-QTOFMS). Identification of the psychoactive component was supported by electron impact gas chromatography/mass spectrometry (GC/EI-MS). The high accuracy of the LC/ESI-QTOFMS method allowed the molecular mass of the investigated substance (M(exp) = 441.0438 Da; mass error, ∆m = 0.2 ppm) and the formulae of ions formed during fragmentation to be determined. The main ions were recorded at m/z = 135.0440, 290.9876 and 305.9981. Structures of the obtained ions were elucidated in the tandem mass spectrometry (MS/MS) experiments by comparing them to mass spectra of previously detected derivatives of phenethylamine. The performed study indicated the potential for using LC/QTOFMS method to identify new designer drugs. This technique can be used supplementary to standard GC/MS. Prior knowledge of the fragmentation mechanisms of phenethylamines allowed to predict the mass spectra of the novel substance--25I-NBMD. Copyright © 2013 John Wiley & Sons, Ltd.

  18. 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.

  19. 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.

  20. Hydrogen atom scrambling in selectively labeled anionic peptides upon collisional activation by MALDI tandem time-of-flight mass spectrometry

    DEFF Research Database (Denmark)

    Bache, Nicolai; Rand, Kasper Dyrberg; Roepstorff, Peter

    2008-01-01

    have now measured the level of hydrogen scrambling in a deprotonated, selectively labeled peptide using MALDI tandem time-of-flight mass spectrometry. Our results conclusively show that hydrogen scrambling is prevalent in the deprotonated peptide upon collisional activation. The amide hydrogens ((1)H....../(2)H) have migrated extensively in the anionic peptide, thereby erasing the original regioselective deuteration pattern obtained in solution....

  1. 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.

  2. [Structure identification of contaminants in a beverage product by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry].

    Science.gov (United States)

    Miyamoto, Yasuhisa; Washida, Kazuto; Uyama, Atsuo; Mochizuki, Naoki

    2014-01-01

    The contaminants in a beverage product that had been reported to have a strange taste were identified. By comparative analysis with the normal product using liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF-MS), six unknown compounds were detected in the total ion current chromatograms of the product in question. Detailed analysis of the mass spectra and product ion spectra of these compounds strongly suggested that the compounds were capric acid diethanolamide, lauric acid diethanolamide, myristic acid diethanolamide, lauryl dimethylaminoacetic acid, lauryl sulfate, and lauric acid, all of which are surfactants commonly used as ingredients of household detergents and shampoos. We searched commercially available detergent products to check for the presence of these six surfactants, and identified products that might have been intentionally or unintentionally mixed into the beverage product after opening.

  3. Metabolic profiling of Hoodia, Chamomile, Terminalia Species and evaluation of commercial preparations using Ultra-High Performance Quadrupole Time of Flight-Mass Spectrometry

    Science.gov (United States)

    Ultra-High Performance-Quadrupole Time of Flight Mass Spectrometr(UHPLC-QToF-MS)profiling has become an impattant tool for identification of marker compounds and generation of metabolic patterns that could be interrogated using chemometric modeling software. Chemometric approaches can be used to ana...

  4. Chemical fingerprint of Ganmaoling granule by double-wavelength ultra high performance liquid chromatography and ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Lou, Qiong; Ye, Xiaolan; Zhou, Yingyi; Li, Hua; Song, Fenyun

    2015-06-01

    A method incorporating double-wavelength ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry was developed for the investigation of the chemical fingerprint of Ganmaoling granule. The chromatographic separations were performed on an ACQUITY UPLC HSS C18 column (2.1 × 50 mm, 1.8 μm) at 30°C using gradient elution with water/formic acid (1%) and acetonitrile at a flow rate of 0.4 mL/min. A total of 11 chemical constituents of Ganmaoling granule were identified from their molecular weight, UV spectra, tandem mass spectrometry data, and retention behavior by comparing the results with those of the reference standards or literature. And 25 peaks were selected as the common peaks for fingerprint analysis to evaluate the similarities among 25 batches of Ganmaoling granule. The results of principal component analysis and orthogonal projection to latent structures discriminant analysis showed that the important chemical markers that could distinguish the different batches were revealed as 4,5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4-O-caffeoylquinic acid. This is the first report of the ultra high performance liquid chromatography chemical fingerprint and component identification of Ganmaoling granule, which could lay a foundation for further studies of Ganmaoling granule. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Quantification, confirmation and screening capability of UHPLC coupled to triple quadrupole and hybrid quadrupole time-of-flight mass spectrometry in pesticide residue analysis.

    Science.gov (United States)

    Grimalt, Susana; Sancho, Juan V; Pozo, Oscar J; Hernández, Félix

    2010-04-01

    The potential of three mass spectrometry (MS) analyzers (triple quadrupole, QqQ; time of flight, TOF; and quadrupole time of flight, QTOF) has been investigated and compared for quantification, confirmation and screening purposes in pesticide residue analysis of fruit and vegetable samples. For this purpose, analytical methodology for multiresidue determination of 11 pesticides, taken as a model, has been developed and validated in nine food matrices for the three mass analyzers coupled to ultra high pressure liquid chromatography. In all cases, limits of quantification around 0.01 mg/kg were reached, fulfilling the most restrictive case of baby-food analysis. Regarding absolute sensitivity, the lower limits of detection were obtained, as expected, for QqQ (100 fg), whereas slightly higher limits (300 fg) were obtained for both TOF and QTOF. Confirmative capacity of each analyzer was studied for each analyte based on the identification points (IPs) criterion, useful for a comprehensive comparison. QTOF mass analyzer showed the highest confirmatory capacity, although QqQ normally led to sufficient number of IPs, even at lower concentration levels. The potential of TOF MS was also investigated for screening purposes. To this aim, around 50 commercial fruits and vegetables samples were analyzed, searching for more than 400 pesticides. TOF MS proved to be an attractive analytical tool for rapid detection and reliable identification of a large number of pesticides thanks to the full spectrum acquisition at accurate mass with satisfactory sensitivity. This process is readily boosted when combined with specialized software packages, together with theoretical exact mass databases. Several pesticides (e.g. carbendazim in citrus and indoxacarb in grape) were detected in the samples. Further unequivocal confirmation of the identity was performed using reference standards and/or QTOF MS/MS experiments. Copyright 2010 John Wiley & Sons, Ltd.

  6. 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.

  7. 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

    2016-09-24

    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.

  8. Verification of protein biomarker specificity for the identification of biological stains by quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Legg, Kevin M; Powell, Roger; Reisdorph, Nichole; Reisdorph, Rick; Danielson, Phillip B

    2017-03-01

    Advances in proteomics technology over the past decade offer forensic serologists a greatly improved opportunity to accurately characterize the tissue source from which a DNA profile has been developed. Such information can provide critical context to evidence and can help to prioritize downstream DNA analyses. Previous proteome studies compiled panels of "candidate biomarkers" specific to each of five body fluids (i.e., peripheral blood, vaginal/menstrual fluid, seminal fluid, urine, and saliva). Here, a multiplex quadrupole time-of-flight mass spectrometry assay has been developed in order to verify the tissue/body fluid specificity the 23 protein biomarkers that comprise these panels and the consistency with which they can be detected across a sample population of 50 humans. Single-source samples of these human body fluids were accurately identified by the detection of one or more high-specificity biomarkers. Recovery of body fluid samples from a variety of substrates did not impede accurate characterization and, of the potential inhibitors assayed, only chewing tobacco juice appeared to preclude the identification of a target body fluid. Using a series of 2-component mixtures of human body fluids, the multiplex assay accurately identified both components in a single-pass. Only in the case of saliva and peripheral blood did matrix effects appear to impede the detection of salivary proteins. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. 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.

  10. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Assessment of benzophenone-4 reactivity with free chlorine by liquid chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Negreira, N; Rodríguez, I; Rodil, R; Cela, R

    2012-09-19

    The stability of the UV filter benzophenone-4 (BP-4) in free chlorine-containing water was investigated, for the first time, by liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS). High mass accuracy and resolution capabilities of this hybrid mass spectrometer were used for the reliable assignation of empirical formulae and chemical structures of BP-4 derivatives. Time-course profiles of the parent compound and its by-products were simultaneously recorded by direct injection of sample aliquots, after quenching the excess of chlorine, in the LC-QqTOF-MS system. At neutral pHs, in excess of chlorine, BP-4 showed a limited stability fitting a pseudo-first-order degradation kinetics. A noticeable reduction in the half-lives of BP-4 was observed when increasing the sample pH between 6 and 8 units and also in presence of bromide traces. The reaction pathway of this UV filter involved a first electrophilic substitution of hydrogen per chlorine (or bromide) in the phenolic ring, followed by oxidation of the carbonyl moiety to an ester group, which induced a further electrophilic substitution in the same aromatic ring. Above reactions were also noticed when mixing a BP-4 containing personal care product with chlorinated tap water and in chlorinated swimming pool and sewage water, previously spiked with a BP-4 standard. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Investigation of cannabis biomarkers and transformation products in waters by liquid chromatography coupled to time of flight and triple quadrupole mass spectrometry.

    Science.gov (United States)

    Boix, Clara; Ibáñez, María; Bijlsma, Lubertus; Sancho, Juan V; Hernández, Félix

    2014-03-01

    11-Nor-9-carboxy-Δ(9)-tetrahydrocannabinol (THC-COOH) is commonly selected as biomarker for the investigation of cannabis consumption through wastewater analysis. The removal efficiency of THC-COOH in wastewater treatment plants (WWTPs) has been reported to vary between 31% and 98%. Accordingly, possible transformation products (TPs) of this metabolite might be formed during treatment processes or in receiving surface water under environmental conditions. In this work, surface water was spiked with THC-COOH and subjected to hydrolysis, chlorination and photo-degradation (both ultraviolet and simulated sunlight) experiments under laboratory-controlled conditions. One hydrolysis, eight chlorination, three ultraviolet photo-degradation and seven sunlight photo-degradation TPs were tentatively identified by liquid chromatography coupled to quadrupole time-of-flight mass spectrometer (LC-QTOF MS). In a subsequent step, THC-COOH and the identified TPs were searched in wastewater samples using LC coupled to tandem mass spectrometry (LC-MS/MS) with triple quadrupole. THC-COOH was found in all influent and effluent wastewater samples analyzed, although at significant lower concentrations in the effluent samples. The removal efficiency of WWTP under study was approximately 86%. Furthermore, THC-COOH was also investigated in several surface waters, and it was detected in 50% of the samples analyzed. Regarding TPs, none were found in influent wastewater, while one hydrolysis and five photo-degradation (simulated sunlight) TPs were detected in effluent and surface waters. The most detected compound, resulting from sunlight photo-degradation, was found in 60% of surface waters analyzed. This fact illustrates the importance of investigating these TPs in the aquatic environment. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Identification of N-nitrosamines in treated drinking water using nanoelectrospray ionization high-field asymmetric waveform ion mobility spectrometry with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhao, Yuan Yuan; Liu, Xin; Boyd, Jessica M; Qin, Feng; Li, Jianjun; Li, Xing-Fang

    2009-01-01

    We report a nanoelectrospray ionization (nESI) with high-field asymmetric waveform ion mobility spectrometry (FAIMS) and tandem mass spectrometry (MS-MS) method for determination of small molecules of m/z 50 to 200 and its potential application in environmental analysis. Integration of nESI with FAIMS and MS-MS combines the advantages of these three techniques into one method. The nESI provides efficient sample introduction and ionization and allows for collection of multiple data from only microliters of samples. The FAIMS provides rapid separation, reduces or eliminates background interference, and improves the signal-to-noise ratio as much as 10-fold over nESI-MS-MS. The tandem quadrupole time-of-flight MS detection provides accurate mass and mass spectral measurements for structural identification. Characteristics of FAIMS compensation voltage (CV) spectra of seven nitrosamines, N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosodi-n-propylamine (NDPA), N-nitrosodi-n-butylamine (NDBA), N-nitrosopiperidine (NPip), and N-nitrosopyrrolidine (NPyr), were analyzed. The optimal CV of the nitrosamines (at DV -4000 V) were: -1.6 V, NDBA; 2.6 V, NDPA; 6.6 V, NPip; 8.8 V, NDEA; 13.2 V, NPyr; 14.4 V, NMEA; and 19.4 V, NDMA. Fragmentation patterns of the seven nitrosamines in the nESI-FAIMS-MS-MS were also obtained. The specific CV and MS-MS spectra resulted in positive identification of NPyr and NPip in a treated water sample, demonstrating the potential application of this technique in environmental analysis.

  14. Structural characterization of monoterpene indole alkaloids in ethanolic extracts of Rauwolfia species by liquid chromatography with quadrupole time-of-flight mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Sunil Kumar; Awantika Singh; Vikas Bajpai; Mukesh Srivastava; Bhim Pratap Singh; Brijesh Kumar

    2016-01-01

    Rauwolfia species (Apocynaceae) are medicinal plants well known worldwide due to its potent bioactive monoterpene indole alkaloids (MIAs) such as reserpine, ajmalicine, ajmaline, serpentine and yohimbine. Reserpine, ajmalicine and ajmaline are powerful antihypertensive, tranquilizing agents used in hypertension. Yohimbine is an aphrodisiac used in dietary supplements. As there is no report on the comparative and comprehensive phytochemical investigation of the roots of Rauwolfia species, we have developed an efficient and reliable liquid chromatography-tandem mass spectrometry (LC–MS/MS) method for ethanolic root extract of Rauwolfia species to elucidate the fragmentation pathways for dereplication of bioactive MIAs using high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (HPLC–ESI–QTOF–MS/MS) in positive ion mode. We identified and established diagnostic fragment ions and fragmentation pathways using reserpine, ajmalicine, ajmaline, serpentine and yohimbine. The MS/MS spectra of reserpine, ajmalicine, and ajmaline showed C-ring-cleavage whereas E-ring cleavage was observed in serpentine via Retro Diels Alder (RDA). A total of 47 bioactive MIAs were identified and characterized on the basis of their molecular formula, exact mass measurements and MS/MS analysis. Reserpine, ajmalicine, ajmaline, serpentine and yohimbine were unambiguously identified by comparison with their authentic standards and other 42 MIAs were tentatively identified and characterized from the roots of Rauwolfia hookeri, Rauwolfia micrantha, Rauwolfia serpentina, Rauwolfia verticillata, Rauwolfia tetraphylla and Rauwolfia vomitoria. Application of LC–MS followed by principal component analysis (PCA) has been successfully used to discriminate among six Rauwolfia species.

  15. Collisional activation by MALDI tandem time-of-flight mass spectrometry induces intramolecular migration of amide hydrogens in protonated peptides

    DEFF Research Database (Denmark)

    Jørgensen, Thomas J D; Bache, Nicolai; Roepstorff, Peter

    2005-01-01

    of doubly protonated peptides that the original regioselective deuterium pattern of these peptides is completely erased (Jørgensen, T. J. D., Gårdsvoll, H., Ploug, M., and Roepstorff, P. (2005) Intramolecular migration of amide hydrogens in protonated peptides upon collisional activation. J. Am. Chem. Soc...... randomization among all exchangeable sites (i.e. all N- and O-linked hydrogens) also occurs upon high energy collisional activation of singly protonated peptides. This intense proton/deuteron traffic precludes the use of MALDI tandem time-of-flight mass spectrometry to obtain reliable information...

  16. Performance optimisation of a new-generation orthogonal-acceleration quadrupole-time-of-flight mass spectrometer.

    Science.gov (United States)

    Bristow, Tony; Constantine, Jill; Harrison, Mark; Cavoit, Fabien

    2008-04-01

    Orthogonal-acceleration quadrupole time-of-flight (oa-QTOF) mass spectrometers, employed for accurate mass measurement, have been commercially available for well over a decade. A limitation of the early instruments of this type was the narrow ion abundance range over which accurate mass measurements could be made with a high degree of certainty. Recently, a new generation of oa-QTOF mass spectrometers has been developed and these allow accurate mass measurements to be recorded over a much greater range of ion abundances. This development has resulted from new ion detection technology and improved electronic stability or by accurate control of the number of ions reaching the detector. In this report we describe the results from experiments performed to evaluate the mass measurement performance of the Bruker micrOTOF-Q, a member of the new-generation oa-QTOFs. The relationship between mass accuracy and ion abundance has been extensively evaluated and mass measurement accuracy remained stable (+/-1.5 m m/z units) over approximately 3-4 orders of magnitude of ion abundance. The second feature of the Bruker micrOTOF-Q that was evaluated was the SigmaFit function of the software. This isotope pattern-matching algorithm provides an exact numerical comparison of the theoretical and measured isotope patterns as an additional identification tool to accurate mass measurement. The smaller the value, the closer the match between theoretical and measured isotope patterns. This information is then employed to reduce the number of potential elemental formulae produced from the mass measurements. A relationship between the SigmaFit value and ion abundance has been established. The results from the study for both mass accuracy and SigmaFit were employed to define the performance criteria for the micrOTOF-Q. This provided increased confidence in the selection of elemental formulae resulting from accurate mass measurements.

  17. Quantitative analysis of veterinary drugs in bovine muscle and milk by liquid chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Saito-Shida, Shizuka; Sakai, Takatoshi; Nemoto, Satoru; Akiyama, Hiroshi

    2017-07-01

    A simple and reliable multiresidue method for quantitative determination of veterinary drugs in bovine muscle and milk using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) was developed. Critical MS parameters such as capillary voltage, cone voltage, collision energy, desolvation gas temperature and extraction mass window were carefully optimised to obtain the best possible sensitivity. Analytical samples were prepared using extraction with acetonitrile and hexane in the presence of anhydrous sodium sulphate and acetic acid, followed by ODS cartridge clean-up. The developed method was validated for 82 veterinary drugs in bovine muscle and milk at spike levels of 0.01 and 0.1 mg kg - 1 . With the exception of cefoperazone and phenoxymethylpenicillin, all these compounds exhibited sufficient signal intensity at 0.01 μg ml -1 (equivalent to 0.01 mg kg - 1 ), indicating the high sensitivity of the developed method. For most targets, the determined accuracies were within 70-120%, with repeatability and reproducibility being below 20% at both levels. Except for sulfathiazole in bovine muscle, no interfering peaks at target compound retention times were detected in the blank extract, indicating that the developed method is highly selective. The absence of sulfathiazole in bovine muscle was confirmed by simultaneous acquisition at low and high collision energies to afford exact masses of molecular adduct and fragment ions. Satisfactory linearity was observed for all compounds, with matrix effects being negligible for most targets in bovine muscle and milk at both spike levels. Overall, the results suggest that the developed LC-QTOF-MS method is suitable for routine regulatory-purpose analysis of veterinary drugs in bovine muscle and milk.

  18. 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.

  19. 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. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  20. Use of liquid chromatography coupled to quadrupole time-of-flight mass spectrometry to investigate pesticide residues in fruits.

    Science.gov (United States)

    Grimalt, Susana; Pozo, Oscar J; Sancho, Juan V; Hernández, Félix

    2007-04-01

    In this paper, the potential of coupling liquid chromatography with hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF) for the determination of pesticides in a variety of fruit samples (orange peel and flesh, banana skin and flesh, strawberry and pear) has been explored. The quantitative application at residue levels has been proven for two insecticides (buprofezin and hexythiazox), which were satisfactorily determined at three concentration levels, 0.1, 1, and 5 mg/kg, obtaining a suitable linearity range (correlation coefficient>0.99) of more than 2 orders of magnitude. Satisfactory recoveries have been obtained for both compounds at the three levels tested in all sample matrices, with lowest calibration levels (LCL) of 0.075 and 0.01 mg/kg. The excellent potential of QTOF for identification purposes is illustrated by the high number of identification points (IPs) earned, up to 21, at the highest concentration of 5 mg/kg, or between 11 and 21 at the 0.1 and 1 mg/kg levels. The application of LC-QTOF MS to real samples revealed the presence of several positives at concentrations close to the LCL, all of which were confirmed with more than 11 IPs. The potential of QTOF for elucidation of nontarget analytes has also been demonstrated by the finding of one transformation product (TP) of buprofezin in a banana skin sample. This TP was identified by obtaining the full scan product ion spectra at different collision energies with acceptable accurate mass deviation. The work performed in this paper illustrates the suitability and excellent confirmatory potential of LC-QTOF MS for pesticides residues analysis in food samples.

  1. Multiple heart-cutting two dimensional liquid chromatography quadrupole time-of-flight mass spectrometry of pyrrolizidine alkaloids.

    Science.gov (United States)

    van de Schans, Milou G M; Blokland, Marco H; Zoontjes, Paul W; Mulder, Patrick P J; Nielen, Michel W F

    2017-06-23

    Pyrrolizidine alkaloids (PAs) and their and the corresponding N-oxides (PAs-ox) are genotoxic plant metabolites which can be present as unwanted contaminants in food products of herbal origin like tea and food supplements. PAs and PAs-ox come in a wide variety of molecular structures including many structural isomers. For toxicity assessment it is important to determine the composition of a sample and to resolve all isomeric PAs and PAs-ox, which is currently not possible in one liquid or gas chromatographic (LC or GC) run. In this study an online two dimensional liquid chromatography quadrupole time-of-flight mass spectrometry (2D-LC QToF-MS) method was developed to resolve isomeric PAs and PAs-ox. After comprehensive column and mobile phase selection a polar endcapped C 18 column was used at pH 3 in the first dimension, and a cross-linked C 18 column at pH 10 in the second dimension. Injection solvents, column IDs, flow rates and temperatures were carefully optimized. The method with column selection valve switching described in this study was able to resolve and visualize 20 individual PAs/PAs-ox (6 sets of isomers) in one 2D-LC QToF-MS run. Moreover, it was shown that all isomeric PAs/PAs-ox could be unambiguously annotated. The method was shown to be applicable for the determination and quantification of isomeric PAs/PAs-ox in plant extracts and could be easily extended to include other PAs and PAs-ox. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. 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. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Application of ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry in identification of three isoflavone glycosides and their corresponding metabolites.

    Science.gov (United States)

    Xu, Xiafen; Li, Xinhui; Liang, Xianrui

    2018-02-15

    Metabolites of isoflavones have attracted much attention in recent years due to their potential bioactivities. However, the complex constituents of the metabolic system and the low level of metabolites make them difficult to analyze. A mass spectrometry (MS) method was applied in our identification of metabolites and study of their fragmentation pathways due to the advantages of rapidity, sensitivity, and low level of sample consumption. Three isoflavone glycosides and their metabolites were identified using ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC/QTOF-MS). These metabolites were obtained by anaerobically incubating three isoflavone glycosides with human intestinal flora. The characteristic fragments of isoflavone glycosides and their metabolites were used for the identification work. Two metabolites from ononin, three metabolites from irilone-4'-O-β-D-glucoside, and five metabolites from sissotrin were identified respectively by the retention time (RT), accurate mass, and mass spectral fragmentation patterns. The losses of the glucosyl group, CO from the [M+H] + ion were observed for all the three isoflavone glycosides. The characteristic retro-Diels-Alder (RDA) fragmentation patterns were used to differentiate the compounds. The metabolic pathways of the three isoflavone glycosides were proposed according to the identified chemical structures of the metabolites. A selective, sensitive and rapid method was established for detecting and identifying three isoflavone glycosides and their metabolites using UPLC/QTOF-MS. The established method can be used for further rapid structural identification studies of metabolites and natural products. Furthermore, the proposed metabolic pathways will be helpful for understanding the in vivo metabolic process of isoflavone. Copyright © 2017 John Wiley & Sons, Ltd.

  4. Ultra high performance liquid chromatography coupled with electrospray ionization/quadrupole time-of-flight mass spectrometry for the rapid analysis of constituents in the traditional Chinese medicine formula Wu Ji Bai Feng Pill.

    Science.gov (United States)

    Duan, Shengnan; Qi, Wen; Zhang, Siwen; Huang, Kunkun; Yuan, Dan

    2017-10-01

    An ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry method in both positive and negative ion modes was established in order to comprehensively investigate the major constituents in Wu Ji Bai Feng Pill. Briefly, a Waters ACQUITY UPLC HSS C 18 column was used to separate the aqueous extract of Wu Ji Bai Feng Pill. A total of 0.1% formic acid in acetonitrile and 0.1% aqueous formic acid v/v were used as the mobile phase. All analytes were determined using quadrupole time-of-flight mass spectrometry with electrospray ionization source in positive and negative ion modes. At length, a total of 173 components including flavones and their glycosides, monoterpene glycosides, triterpene saponins, phenethylalchohol glycosides, iridoid glycosides, phthalides, tanshinones, phenolic acids, sesquiterpenoids and cyclopeptides were identified or tentatively characterized in Wu Ji Bai Feng Pill in an analysis of 16.0 min based on the accurate mass and tandem mass spectrometry behaviors. The developed method is rapid and highly sensitive to characterize the chemical constituents of Wu Ji Bai Feng Pill, which could not only be used for chemical standardization and quality control of Wu Ji Bai Feng Pill, but also be helpful for further study in vivo metabolism of Wu Ji Bai Feng Pill. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Determination of thyroid hormones in placenta using isotope-dilution liquid chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Li, Zhong-Min; Giesert, Florian; Vogt-Weisenhorn, Daniela; Main, Katharina Maria; Skakkebæk, Niels Erik; Kiviranta, Hannu; Toppari, Jorma; Feldt-Rasmussen, Ulla; Shen, Heqing; Schramm, Karl-Werner; De Angelis, Meri

    2018-01-26

    The transplacental passage of thyroid hormones (THs) is of great significance since the maternal THs are vitally important in ensuring the normal fetal development. In this paper, we determined the concentrations of seven THs, viz. L-thyroxine (T 4 ), 3,3',5-triiodo-l-thyronine (T 3 ), 3,3',5'-triiodo-l-thyronine (rT 3 ), 3,3'-diiodo-l-thyronine (T 2 ), 3,5-diiodo-l-thyronine (rT 2 ), 3-iodo-l-thyronine (T 1 ) and 3-iodothyronamine (T 1 AM), in placenta using isotope dilution liquid chromatography quadrupole time-of-flight mass spectrometry. We optimized the method using isotopically labeled quantification standards ( 13 C 6 -T 4 , 13 C 6 -T 3 , 13 C 6 -rT 3 and 13 C 6 -T 2 ) and recovery standard ( 13 C 12 -T 4 ) in combination with solid-liquid extraction, liquid-liquid extraction and solid phase extraction. The linearity was obtained in the range of 0.5-150 pg uL -1 with R 2 values >0.99. The method detection limits (MDLs) ranged from 0.01 ng g -1 to 0.2 ng g -1 , while the method quantification limits (MQLs) were between 0.04 ng g -1 and 0.7 ng g -1 . The spike-recoveries for THs (except for T 1 and T 1 AM) were in the range of 81.0%-112%, with a coefficient of variation (CV) of 0.5-6.2%. The intra-day CVs and inter-day CVs were 0.5%-10.3% and 1.19%-8.88%, respectively. Concentrations of the THs were 22.9-35.0 ng g -1  T 4 , 0.32-0.46 ng g -1  T 3 , 2.86-3.69 ng g -1 rT 3 , 0.16-0.26 ng g -1  T 2 , and < MDL for other THs in five human placentas, and 2.05-3.51 ng g -1  T 4 , 0.37-0.62 ng g -1  T 3 , 0.96-1.3 ng g -1 rT 3 , 0.07-0.13 ng g -1  T 2 and < MDL for other THs in five mouse placentas. The presence of T 2 was tracked in placenta for the first time. This method with improved selectivity and sensitivity allows comprehensive evaluation of TH homeostasis in research of metabolism and effects of environmental contaminant exposures. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Bioactivity evaluation-based ultra high-performance liquid chromatography coupled with electrospray ionization tandem quadrupole-time-of-flight mass spectrometry and novel distinction of multi-subchemome compatibility recognition strategy with Astragali Radix-Fructus Corni herb-pair as a case study.

    Science.gov (United States)

    Duan, Yu; Pei, Ke; Cai, Hao; Tu, Sicong; Zhang, Zhengwei; Cheng, Xinwei; Qiao, Fengxian; Fan, Kailei; Qin, Kunming; Liu, Xiao; Cai, Baochang

    2016-09-10

    The approach to investigate traditional Chinese medicine (TCM) is still in its infancy and has been facing enormous challenge. In this paper, a generally applicable strategy was developed for investigation on TCM systematically with an introduced interesting idea about a novel research system which called subchemome. A representative herb-pair, Astragali Radix-Fructus Corni, was successfully employed to expound this novel strategy. Firstly, subchemomes were prepared individually by applying the suitable column chromatography, each of them was detected by UV spectrophotometer or HPLC-DAD detector. The components in each part were then identified based on the mass spectrometric fragmentation patterns and tandem mass spectrometric data by using UHPLC-Q-TOF-MS. Using renal mesangial cell (RMC) viability assay as the evaluation of the pharmacological activity of each group, we developed the new mini herbal formulae aimed at diabetic nephropathy and identified fifteen marker components between the group of new mini herbal formulae and other groups from the angle of the constituent, and then explored the effects of new mini herbal formulae from another angle of the molecular mechanism. Overall, the presently developed strategy should be beneficial and widely used in the investigation on TCM from a new perspective. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. 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. Published in 2011 by John Wiley & Sons, Ltd.

  9. Multi-constituent determination and fingerprint analysis of Scutellaria indica L. using ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Liang, Xianrui; Zhao, Cui; Su, Weike

    2015-11-01

    An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method integrating multi-constituent determination and fingerprint analysis has been established for quality assessment and control of Scutellaria indica L. The optimized method possesses the advantages of speediness, efficiency, and allows multi-constituents determination and fingerprint analysis in one chromatographic run within 11 min. 36 compounds were detected, and 23 of them were unequivocally identified or tentatively assigned. The established fingerprint method was applied to the analysis of ten S. indica samples from different geographic locations. The quality assessment was achieved by using principal component analysis. The proposed method is useful and reliable for the characterization of multi-constituents in a complex chemical system and the overall quality assessment of S. indica. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Profiling of nonvolatiles in whiskeys using ultra high pressure liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS).

    Science.gov (United States)

    Collins, Thomas S; Zweigenbaum, Jerry; Ebeler, Susan E

    2014-11-15

    Commercial samples of 63 American whiskeys, including bourbon whiskeys, Tennessee whiskeys, rye whiskeys and other blended whiskeys were analysed using ultra high pressure liquid chromatography (UHPLC) coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS). The non-volatile composition of the whiskeys was used to model differences among the samples using discriminant analysis. The blended American whiskeys were readily distinguished from the remaining types. Additionally, most Tennessee whiskeys could be differentiated from bourbon and rye whiskeys. Similarly, younger (8 years old) whiskeys could be separated. The compounds important for differentiating among these whiskeys included wood derived phenolic compounds, lignan derived compounds and several C8 and larger lipids. A number of additional compounds differentiated the whiskeys but could not be identified using MS and MS/MS data alone. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Untargeted metabolomic analysis using liquid chromatography quadrupole time-of-flight mass spectrometry for non-volatile profiling of wines

    International Nuclear Information System (INIS)

    Arbulu, M.; Sampedro, M.C.; Gómez-Caballero, A.; Goicolea, M.A.; Barrio, R.J.

    2015-01-01

    Highlights: • An untargeted metabolomic method for the non-volatile profile of the Graciano wine was developed. • 411 different metabolites in Graciano Vitis vinifera red wine were identified. • 15 compounds could serve to differentiate Graciano and Tempranillo wines. • An enological database (WinMet) with 2080 compounds was constructed. - Abstract: The current study presents a method for comprehensive untargeted metabolomic fingerprinting of the non-volatile profile of the Graciano Vitis vinifera wine variety, using liquid chromatography/electrospray ionization time of flight mass spectrometry (LC–ESI-QTOF). Pre-treatment of samples, chromatographic columns, mobile phases, elution gradients and ionization sources, were evaluated for the extraction of the maximum number of metabolites in red wine. Putative compounds were extracted from the raw data using the extraction algorithm, molecular feature extractor (MFE). For the metabolite identification the WinMet database was designed based on electronic databases and literature research and includes only the putative metabolites reported to be present in oenological matrices. The results from WinMet were compared with those in the METLIN database to evaluate how much the databases overlap for performing identifications. The reproducibility of the analysis was assessed using manual processing following replicate injections of Vitis vinifera cv. Graciano wine spiked with external standards. In the present work, 411 different metabolites in Graciano Vitis vinifera red wine were identified, including primary wine metabolites such as sugars (4%), amino acids (23%), biogenic amines (4%), fatty acids (2%), and organic acids (32%) and secondary metabolites such as phenols (27%) and esters (8%). Significant differences between varieties Tempranillo and Graciano were related to the presence of fifteen specific compounds

  12. Untargeted metabolomic analysis using liquid chromatography quadrupole time-of-flight mass spectrometry for non-volatile profiling of wines

    Energy Technology Data Exchange (ETDEWEB)

    Arbulu, M. [Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country, 01006 Vitoria-Gasteiz (Spain); Sampedro, M.C. [Central Service of Analysis, SGIker, University of the Basque Country, 01006 Vitoria-Gasteiz (Spain); Gómez-Caballero, A.; Goicolea, M.A. [Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country, 01006 Vitoria-Gasteiz (Spain); Barrio, R.J., E-mail: r.barrio@ehu.es [Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country, 01006 Vitoria-Gasteiz (Spain)

    2015-02-09

    Highlights: • An untargeted metabolomic method for the non-volatile profile of the Graciano wine was developed. • 411 different metabolites in Graciano Vitis vinifera red wine were identified. • 15 compounds could serve to differentiate Graciano and Tempranillo wines. • An enological database (WinMet) with 2080 compounds was constructed. - Abstract: The current study presents a method for comprehensive untargeted metabolomic fingerprinting of the non-volatile profile of the Graciano Vitis vinifera wine variety, using liquid chromatography/electrospray ionization time of flight mass spectrometry (LC–ESI-QTOF). Pre-treatment of samples, chromatographic columns, mobile phases, elution gradients and ionization sources, were evaluated for the extraction of the maximum number of metabolites in red wine. Putative compounds were extracted from the raw data using the extraction algorithm, molecular feature extractor (MFE). For the metabolite identification the WinMet database was designed based on electronic databases and literature research and includes only the putative metabolites reported to be present in oenological matrices. The results from WinMet were compared with those in the METLIN database to evaluate how much the databases overlap for performing identifications. The reproducibility of the analysis was assessed using manual processing following replicate injections of Vitis vinifera cv. Graciano wine spiked with external standards. In the present work, 411 different metabolites in Graciano Vitis vinifera red wine were identified, including primary wine metabolites such as sugars (4%), amino acids (23%), biogenic amines (4%), fatty acids (2%), and organic acids (32%) and secondary metabolites such as phenols (27%) and esters (8%). Significant differences between varieties Tempranillo and Graciano were related to the presence of fifteen specific compounds.

  13. 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.

  14. 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.

  15. A peptidomic approach for monitoring and characterising peptide cyanotoxins produced in Italian lakes by matrix-assisted laser desorption/ionisation and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Ferranti, Pasquale; Nasi, Antonella; Bruno, Milena; Basile, Adriana; Serpe, Luigi; Gallo, Pasquale

    2011-05-15

    In recent years, the occurrence of cyanobacterial blooms in eutrophic freshwaters has been described all over the world, including most European countries. Blooms of cyanobacteria may produce mixtures of toxic secondary metabolites, called cyanotoxins. Among these, the most studied are microcystins, a group of cyclic heptapeptides, because of their potent hepatotoxicity and activity as tumour promoters. Other peptide cyanotoxins have been described whose structure and toxicity have not been thoroughly studied. Herein we present a peptidomic approach aimed to characterise and quantify the peptide cyanotoxins produced in two Italian lakes, Averno and Albano. The procedure was based on matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry mass spectrometry (MALDI-TOF-MS) analysis for rapid detection and profiling of the peptide mixture complexity, combined with liquid chromatography/electrospray ionisation quadrupole time-of- flight tandem mass spectrometry (LC/ESI-Q-TOF-MS/MS) which provided unambiguous structural identification of the main compounds, as well as accurate quantitative analysis of microcystins. In the case of Lake Averno, a novel variant of microcystin-RR and two novel anabaenopeptin variants (Anabaenopeptins B(1) and Anabaenopeptin F(1)), presenting homoarginine in place of the commonly found arginine, were detected and characterised. In Lake Albano, the peculiar peptide patterns in different years were compared, as an example of the potentiality of the peptidomic approach for fast screening analysis, prior to fine structural analysis and determination of cyanotoxins, which included six novel aeruginosin variants. This approach allows for wide range monitoring of cyanobacteria blooms, and to collect data for evaluating possible health risks to consumers, through the panel of the compounds produced along different years. Copyright © 2011 John Wiley & Sons, Ltd.

  16. 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

  17. A novel approach to the quantitative detection of anabolic steroids in bovine muscle tissue by means of a hybrid quadrupole time-of-flight-mass spectrometry instrument.

    Science.gov (United States)

    Bussche, Julie Vanden; Decloedt, Anneleen; Van Meulebroek, Lieven; De Clercq, Nathalie; Lock, Stephen; Stahl-Zeng, Jianru; Vanhaecke, Lynn

    2014-09-19

    In recent years, the analysis of veterinary drugs and growth-promoting agents has shifted from target-oriented procedures, mainly based on liquid chromatography coupled to triple-quadrupole mass spectrometry (LC-QqQ-MS), towards accurate mass full scan MS (such as Time-of-Flight (ToF) and Fourier Transform (FT)-MS). In this study, the performance of a hybrid analysis instrument (i.e. UHPLC-QuadrupoleTime-of-Flight-MS (QqToF-MS)), able to exploit both full scan HR and MS/MS capabilities within a single analytical platform, was evaluated for confirmatory analysis of anabolic steroids (gestagens, estrogens including stilbenes and androgens) in meat. The validation data was compared to previously obtained results (CD 2002/657/EC) for QqQ-MS and single stage Orbitrap-MS. Additionally, a fractional factorial design was used to shorten and optimize the sample extraction. Validation according to CD 2002/657/EC demonstrated that steroid analysis using QqToF has a higher competing value towards QqQ-MS in terms of selectivity/specificity, compared to single stage Orbitrap-MS. While providing excellent linearity, based on lack-of-fit calculations (F-test, α=0.05 for all steroids except 17β-ethinylestradiol: α=0.01), the sensitivity of QqToF-MS proved for 61.8% and 85.3% of the compounds more sensitive compared to QqQ-MS and Orbitrap-MS, respectively. Indeed, the CCα values, obtained upon ToF-MS/MS detection, ranged from 0.02 to 1.74μgkg(-1) for the 34 anabolic steroids, while for QqQ-MS and Orbitrap-MS values ranged from 0.04 to 0.88μgkg(-1) and from 0.07 to 2.50μgkg(-1), respectively. Using QqToF-MS and QqQ-MS, adequate precision was obtained as relative standard deviations for repeatability and within-laboratory reproducibility, were below 20%. In case of Orbitrap-MS, some compounds (i.e. some estrogens) displayed poor precision, which was possibly caused by some lack of sensitivity at lower concentrations and the absence of MRM-like experiments. Overall, it can be

  18. Identification of metabolites in human and rat urine after oral administration of Xiao-Qing-Long-Tang granule using ultra high performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhou, Lei; Zhang, Qiang; Qi, Wen; Yan, Shuai; Qu, Jialin; Makino, Toshiaki; Yuan, Dan

    2017-09-01

    Xiao-Qing-Long-Tang is a traditional Chinese formula used for the treatment of cold syndrome, bronchitis, and nasal allergies for thousands of years. However, the in vivo integrated metabolism of its multiple components and the active chemical constituents of Xiao-Qing-Long-Tang remain unknown. In this study, a method using ultra high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry was established for the detection and identification of the metabolites in human and rat urine after oral administration of Xiao-Qing-Long-Tang. A total of 19 compounds were detected or tentatively identified in human urine samples, including eight prototypes and 11 metabolites. Also, a total of 50 compounds were detected or tentatively identified in rat urine samples, including 15 prototypes and 35 metabolites detected with either a highly sensitive extracted ion chromatogram method or the MS E determination using Mass Fragment software. Our results indicated that phase Ⅱ reactions (e.g. glucuronidation and sulfation) were the main metabolic pathways of flavones, while phase I reactions (e.g. demethylation and hydroxylation) were the major metabolic reaction for alkaloids, lignans, and ginger essential oil. This investigation provided important structural information on the metabolism of Xiao-Qing-Long-Tang and provided evidence to obtain a more comprehensive metabolic profile. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Antioxidant activity and ultra-performance LC-electrospray ionization-quadrupole time-of-flight mass spectrometry for phenolics-based fingerprinting of Rose species: Rosa damascena, Rosa bourboniana and Rosa brunonii.

    Science.gov (United States)

    Kumar, Neeraj; Bhandari, Pamita; Singh, Bikram; Bari, Shamsher S

    2009-02-01

    Roses are one of the most important groups of ornamental plants and their fruits and flowers are used in a wide variety of food, nutritional products and different traditional medicines. The antioxidant activity of methanolic extracts from fresh flowers of three rose species (Rosa damascena, Rosa bourboniana and Rosa brunonii) was evaluated by 1,1-diphenyl-2-picryl hydrazyl (DPPH) free-radical method. The ability to scavenge DPPH radical was measured by the discoloration of the solution. The methanolic extract from R. brunonii exhibited maximum free-radical-scavenging activity (64.5+/-0.38%) followed by R. bourboniana (51.8+/-0.46%) and R. damascena (43.6+/-0.25%) at 100 microg/ml. Simultaneously, ultra-performance liquid chromatography coupled with electrospray ionization-quadrupole time-of-flight mass spectrometry (UPLC-ESI-QTOF-MS) was used to study phenolic composition in the methanolic extracts from the fresh flowers of rose species. The phenolic constituents were further investigated by direct infusion-ESI-QTOF-MS/MS in negative ion mode. Characteristic Electrospray ionization tandem mass spectrometry (ESI-MS/MS) spectra with other diagnostic fragment ions generated by retro Diels-Alder (RDA) fragmentation pathways were recorded for the flavonoids. Distinct similarities were observed in the relative distribution of polyphenolic compounds among the three species. The dominance of quercetin, kaempferol and their glycosides was observed in all the three species.

  20. Quantitative analysis of flavanones from citrus fruits by using mesoporous molecular sieve-based miniaturized solid phase extraction coupled to ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Cao, Wan; Ye, Li-Hong; Cao, Jun; Xu, Jing-Jing; Peng, Li-Qing; Zhu, Qiong-Yao; Zhang, Qian-Yun; Hu, Shuai-Shuai

    2015-08-07

    An analytical procedure based on miniaturized solid phase extraction (SPE) and ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry was developed and validated for determination of six flavanones in Citrus fruits. The mesoporous molecular sieve SBA-15 as a solid sorbent was characterised by Fourier transform-infrared spectroscopy and scanning electron microscopy. Additionally, compared with reported extraction techniques, the mesoporous SBA-15 based SPE method possessed the advantages of shorter analysis time and higher sensitivity. Furthermore, considering the different nature of the tested compounds, all of the parameters, including the SBA-15 amount, solution pH, elution solvent, and the sorbent type, were investigated in detail. Under the optimum condition, the instrumental detection and quantitation limits calculated were less than 4.26 and 14.29ngmL(-1), respectively. The recoveries obtained for all the analytes were ranging from 89.22% to 103.46%. The experimental results suggested that SBA-15 was a promising material for the purification and enrichment of target flavanones from complex citrus fruit samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Cyclodextrin-based miniaturized solid phase extraction for biopesticides analysis in water and vegetable juices samples analyzed by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Peng, Li-Qing; Ye, Li-Hong; Cao, Jun; Chang, Yan-Xu; Li, Qin; An, Mingrui; Tan, Zhijing; Xu, Jing-Jing

    2017-07-01

    A cyclodextrin-based miniaturized solid-phase extraction was developed to extract biopesticides from water and vegetable juices. The analytes were detected by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. In the solid-phase extraction (SPE) procedure, the liquid sample solution is passed through a packed column filled with 40mg of HP-β-CD, and then the target analytes are absorbed and finally eluted with methanol-acetic acid (90:10, v/v) into a collection tube. The limits of quantification ranged from 3.73 to 16.51ng/mL for a water matrix, from 2.62 to 13.23ng/mL for an orange juice matrix and from 1.76 to 10.35ng/mL for a tomato juice matrix, respectively. The average recovery values were in the range of 88.3-95.9% for the spiked samples. The established methodology was successfully applied to analyze sanguinarine, berberine, rotenone and osthole in water, orange juice and tomato juice. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Metabolomics study on primary dysmenorrhea patients during the luteal regression stage based on ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry

    Science.gov (United States)

    Fang, Ling; Gu, Caiyun; Liu, Xinyu; Xie, Jiabin; Hou, Zhiguo; Tian, Meng; Yin, Jia; Li, Aizhu; Li, Yubo

    2017-01-01

    Primary dysmenorrhea (PD) is a common gynecological disorder which, while not life-threatening, severely affects the quality of life of women. Most patients with PD suffer ovarian hormone imbalances caused by uterine contraction, which results in dysmenorrhea. PD patients may also suffer from increases in estrogen levels caused by increased levels of prostaglandin synthesis and release during luteal regression and early menstruation. Although PD pathogenesis has been previously reported on, these studies only examined the menstrual period and neglected the importance of the luteal regression stage. Therefore, the present study used urine metabolomics to examine changes in endogenous substances and detect urine biomarkers for PD during luteal regression. Ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry was used to create metabolomic profiles for 36 patients with PD and 27 healthy controls. Principal component analysis and partial least squares discriminate analysis were used to investigate the metabolic alterations associated with PD. Ten biomarkers for PD were identified, including ornithine, dihydrocortisol, histidine, citrulline, sphinganine, phytosphingosine, progesterone, 17-hydroxyprogesterone, androstenedione, and 15-keto-prostaglandin F2α. The specificity and sensitivity of these biomarkers was assessed based on the area under the curve of receiver operator characteristic curves, which can be used to distinguish patients with PD from healthy controls. These results provide novel targets for the treatment of PD. PMID:28098892

  3. Fenofibrate Metabolism in the Cynomolgus Monkey using Ultraperformance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry-Based MetabolomicsS⃞

    Science.gov (United States)

    Liu, Aiming; Patterson, Andrew D.; Yang, Zongtao; Zhang, Xinying; Liu, Wei; Qiu, Fayang; Sun, He; Krausz, Kristopher W.; Idle, Jeffrey R.; Gonzalez, Frank J.; Dai, Renke

    2009-01-01

    Fenofibrate, widely used for the treatment of dyslipidemia, activates the nuclear receptor, peroxisome proliferator-activated receptor α. However, liver toxicity, including liver cancer, occurs in rodents treated with fibrate drugs. Marked species differences occur in response to fibrate drugs, especially between rodents and humans, the latter of which are resistant to fibrate-induced cancer. Fenofibrate metabolism, which also shows species differences, has not been fully determined in humans and surrogate primates. In the present study, the metabolism of fenofibrate was investigated in cynomolgus monkeys by ultraperformance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOFMS)-based metabolomics. Urine samples were collected before and after oral doses of fenofibrate. The samples were analyzed in both positive-ion and negative-ion modes by UPLC-QTOFMS, and after data deconvolution, the resulting data matrices were subjected to multivariate data analysis. Pattern recognition was performed on the retention time, mass/charge ratio, and other metabolite-related variables. Synthesized or purchased authentic compounds were used for metabolite identification and structure elucidation by liquid chromatographytandem mass spectrometry. Several metabolites were identified, including fenofibric acid, reduced fenofibric acid, fenofibric acid ester glucuronide, reduced fenofibric acid ester glucuronide, and compound X. Another two metabolites (compound B and compound AR), not previously reported in other species, were characterized in cynomolgus monkeys. More importantly, previously unknown metabolites, fenofibric acid taurine conjugate and reduced fenofibric acid taurine conjugate were identified, revealing a previously unrecognized conjugation pathway for fenofibrate. PMID:19251819

  4. Early Metabolome Profiling and Prognostic Value in Paraquat-Poisoned Patients: Based on Ultraperformance Liquid Chromatography Coupled To Quadrupole Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Hu, Lufeng; Hong, Guangliang; Tang, Yahui; Wang, Xianqin; Wen, Congcong; Lin, Feiyan; Lu, Zhongqiu

    2017-12-18

    Paraquat (PQ) has caused countless deaths throughout the world. There remains no effective treatment for PQ poisoning. Here we study the blood metabolome of PQ-poisoned patients using ultraperformance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS). Patients were divided into groups according to blood PQ concentration. Healthy subjects served as controls. Metabolic features were statistically analyzed using multivariate pattern-recognition techniques to identify the most important metabolites. Selected metabolites were further compared with a series of clinical indexes to assess the prognostic value. PQ-poisoned patients showed substantial differences compared with healthy subjects. Based on variable of importance in the project (VIP) values and statistical analysis, 17 metabolites were selected and identified. These metabolites well-classified low PQ-poisoned patients, high PQ-poisoned patients, and healthy subjects, which was better than that of a complete blood count (CBC). Among the 17 metabolites, 20:3/18:1-PC (PC), LPA (0:0/16:0) (LPA), 19-oxo-deoxycorticosterone (19-oxo-DOC), and eicosapentaenoic acid (EPA) had prognostic value. In particular, EPA was the most sensitive one. Besides, the levels of EPA was correlated with LPA and 19-oxo-DOC. If EPA was excessively consumed, then prognosis was poor. In conclusion, the serum metabolome is substantially perturbed by PQ poisoning. EPA is the most important biomarker in early PQ poisoning.

  5. Multi-ingredients determination and fingerprint analysis of leaves from Ilex latifolia using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Fan, Chunlin; Deng, Jiewei; Yang, Yunyun; Liu, Junshan; Wang, Ying; Zhang, Xiaoqi; Fai, Kuokchiu; Zhang, Qingwen; Ye, Wencai

    2013-10-01

    An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) method integrating multi-ingredients determination and fingerprint analysis has been established for quality assessment and control of leaves from Ilex latifolia. The method possesses the advantages of speediness, efficiency, accuracy, and allows the multi-ingredients determination and fingerprint analysis in one chromatographic run within 13min. Multi-ingredients determination was performed based on the extracted ion chromatograms of the exact pseudo-molecular ions (with a 0.01Da window), and fingerprint analysis was performed based on the base peak chromatograms, obtained by negative-ion electrospray ionization QTOF-MS. The method validation results demonstrated our developed method possessing desirable specificity, linearity, precision and accuracy. The method was utilized to analyze 22 I. latifolia samples from different origins. The quality assessment was achieved by using both similarity analysis (SA) and principal component analysis (PCA), and the results from SA were consistent with those from PCA. Our experimental results demonstrate that the strategy integrated multi-ingredients determination and fingerprint analysis using UPLC-QTOF-MS technique is a useful approach for rapid pharmaceutical analysis, with promising prospects for the differentiation of origin, the determination of authenticity, and the overall quality assessment of herbal medicines. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Determination of sildenafil mixed into herbal honey mixture by ultra-performance liquid chromatography-quadrupole time of flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    Neira Mustabasic

    2017-01-01

    Full Text Available There has been a number of reports of natural products contaminated with illegal adulterants that threaten consumer health because of their adverse pharmacological effects worldwide. In this study, a multi-residual ultra-performance liquid chromatography method with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS was applied for the identification of sildenafil added into a herbal honey mixture used as an immune system booster. Electrospray ionization (ESI source was applied and operated in the positive ion mode. The mobile phase consisted of 0.1% formic acid aqueous solution/acetonitrile (70:30, v/v using the isocratic gradient elution system at a detection wavelength of 290 nm. The compound of sildenafil added into traditional herbal mixed honey was identified according to the spectrum, chromatographic behavior, and mass spectral data were identified by comparison with the reference substance. The method is selective, sensitive and can be used to detect the sildenafil illegally added into traditional herbal medicinal preparations.

  7. Identification of metabolites of Helicid in vivo using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Diao, Xinpeng; Liao, Man; Cheng, Xiaoye; Liang, Caijuan; Sun, Yupeng; Zhang, Xia; Zhang, Lantong

    2018-04-18

    Helicid is an active natural aromatic phenolic glycoside ingredient originating from well-known traditional Chinese herb medicine and has the significant effects of sedative hypnosis, anti-inflammatory analgesia and antidepressant. In this study, we analyzed the potential metabolites of Helicid in rats by multiple mass defect filter (MMDF)and dynamic background subtraction (DBS)in ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS). Moreover, we used a novel data processing method 'key product ions (KPIs)' to rapidly detect and identifymetabolites as an assistant tool. MetabolitePilot TM 2.0 software and PeakView TM 2.2 software were used for analyzing metabolites. Twenty metabolites of Helicid (including 15 phase I metabolites and 5 phase II metabolites) were detected by comparing with the blank samples, respectively. Thebiotransformationroute of Helicid was identified as demethylation, oxidation, dehydroxylation, hydrogenation, decarbonylation,glucuronide conjugation and methylation.This is the first study of simultaneously detecting and identifying Helicid metabolism in rats by employing UHPLC-Q-TOF-MS technology. This experiment not only proposed a method for rapidly detecting and identifying metabolites, but also provided useful information for further study of the pharmacology and mechanism of Helicid in vivo. Furthermore, it provided an effective method for the analysis of other aromatic phenolic glycosides metabolic components in vivo. This article is protected by copyright. All rights reserved.

  8. Identification of berberrubine metabolites in rats by using ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Kun; Qiao, Miao; Chai, Liwei; Cao, Shijie; Feng, Xinchi; Ding, Liqin; Qiu, Feng

    2018-01-01

    Berberrubine, an isoquinoline alkaloid isolated from many medicinal plants, possesses diverse pharmacological activities, including glucose-lowering, lipid-lowering, anti-inflammatory, and anti-tumor effects. This study aimed to investigate the metabolic profile of berberrubine in vivo. Therefore, a rapid and reliable method using the ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and metabolynx™ software with mass defect filter (MDF) technique was developed. Plasma, bile, urine and feces samples were collected from rats after oral administration of berberrubine with a dose of 30.0mg/kg and analyzed to characterize the metabolites of berberrubine in vivo for the first time. A total of 57 metabolites were identified, including 54 metabolites in urine, 39 metabolites in plasma, 28 metabolites in bile and 18 metabolites in feces. The results indicated that demethylenation, reduction, hydroxylation, demethylation, glucuronidation, and sulfation were the major metabolic pathways of berberrubine in vivo. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Multi-analysis strategy for metabolism of Andrographis paniculata in rat using liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Li, Wenlan; Sun, Xiangming; Xu, Ying; Wang, Xuezhi; Bai, Jing; Ji, Yubin

    2015-07-01

    Compared with chemical drugs, it is a huge challenge to identify active ingredients of multicomponent traditional Chinese medicine (TCM). For most TCMs, metabolism investigation of absorbed constituents is a feasible way to clarify the active material basis. Although Andrographis paniculata (AP) has been extensively researched by domestic and foreign scholars, its metabolism has seldom been fully addressed to date. In this paper, high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry was applied to analysis and characterization of AP metabolism in rat urine and feces samples after oral administration of ethanol extract. The differences in metabolites and metabolic pathways between the two biological samples were further compared. The chemical structures of 20 components were tentatively identified from drug-treated biological samples, including six prototype components and 14 metabolites, which underwent such main metabolic pathways as hydrolyzation, hydrogenation, dehydroxylation, deoxygenation, methylation, glucuronidation, sulfonation and sulfation. Two co-existing components were found in urine and feces samples, suggesting that some ingredients' metabolic processes were not unique. This study provides a comprehensive report on the metabolism of AP in rats, which will be helpful for understanding its mechanism. Copyright © 2014 John Wiley & Sons, Ltd.

  10. Simultaneous determination of organophosphorus pesticides in fruits and vegetables using atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry.

    Science.gov (United States)

    Cheng, Zhipeng; Dong, Fengshou; Xu, Jun; Liu, Xingang; Wu, Xiaohu; Chen, Zenglong; Pan, Xinglu; Gan, Jay; Zheng, Yongquan

    2017-09-15

    This paper describes the application of atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for the simultaneous determination of organophosphorus pesticides in apple, pear, tomato, cucumber and cabbage. Soft ionization with atmospheric pressure ionization source was compared with traditional electron impact ionization (EI). The sensitivity of GC coupled to atmospheric pressure ionization (APGC) for all the analytes was enhanced by 1.0-8.2 times. The ionization modes with atmospheric pressure ionization source was studied by comparing the charge-transfer and proton-transfer conditions. The optimized QuEChERs method was used to pretreat the samples. The calibration curves were found linear from 10 to 1000μg/L, obtaining correlation coefficients higher than 0.9845. Satisfactory mean recovery values, in the range of 70.0-115.9%, and satisfactory precision, with all RSD r <19.7% and all RSD R values <19.5% at the three fortified concentration levels for all the fifteen OPPs. The results demonstrate the potential of APGC-QTOF-MS for routine quantitative analysis of organophosphorus pesticide in fruits and vegetables. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. A Metabonomics Profiling Study on Phlegm Syndrome and Blood-Stasis Syndrome in Coronary Heart Disease Patients Using Liquid Chromatography/Quadrupole Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Linlin Zhao

    2014-01-01

    Full Text Available A metabonomics approach based on liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS was utilized to obtain potential biomarkers of coronary heart disease (CHD patients and investigate the ZHENG types differentiation in CHD patients. The plasma samples of 20 CHD patients with phlegm syndrome, 20 CHD patients with blood-stasis syndrome, and 16 healthy volunteers were collected in the study. 26 potential biomarkers were identified in the plasma of CHD patients and 19 differential metabolites contributed to the discrimination of phlegm syndrome and blood-stasis syndrome in CHD patients (VIP>1.5; P<0.05 which mainly involved purine metabolism, pyrimidine metabolism, amino acid metabolism, steroid biosynthesis, and arachidonic acid metabolism. This study demonstrated that metabonomics approach based on LC-MS was useful for studying pathologic changes of CHD patients and interpreting the differentiation of ZHENG types (phlegm and blood-stasis syndrome in traditional Chinese medicine (TCM.

  12. A Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry (LC-Q-TOF MS) Study for Analyzing 35 Corticosteroid Compounds: Elucidation of MS/MS Fragmentation Pathways

    International Nuclear Information System (INIS)

    Noh, Eunyoung; Yoon, Chang-Yong; Lee, Ji Hyun; Baek, Sun-Young; Do, Jung-Ah; Lee, Jung-min; Oh, Han Bin

    2016-01-01

    Corticosteroids have been often found to be added to a dietary supplement for the purpose of illegally improving the effect of their products. Thus, it is imperative to develop or improve a method that enables one to rapidly and reliably analyze corticosteroids in health or dietary supplements, for the safety management purpose. In the present study, results from liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS) experiments for the selected 35 corticosteroid compounds are presented, which can be useful for the qualitative screening of corticosteroids in health or dietary supplements. Specifically, retention times, accurate mass data of the protonated steroids, m/z values of major fragment ions are given for the 35 corticosteroids. Further, fragmentation pathways for the selected steroids are also suggested. Based on the suggested fragmentation pathways, it was shown that an unknown steroid compound can be readily identified using the knowledge of a group of unique and specific common skeletal fragments. The high selectivity and sensitivity of the LC-Q-TOF-MS/MS results combined with the knowledge of the fragmentation pathways can offer a new opportunity for rapid and accurate screening of corticosteroids, thus preventing health-related incidents involving adulterated products and clamping down on illegally circulated health products.

  13. In Vitro and in Vivo Metabolite Profiling of Valnemulin Using Ultraperformance Liquid Chromatography–Quadrupole/Time-of-Flight Hybrid Mass Spectrometry

    Science.gov (United States)

    2015-01-01

    Valnemulin, a semisynthetic pleuromutilin derivative related to tiamulin, is broadly used to treat bacterial diseases of animals. Despite its widespread use, metabolism in animals has not yet been fully investigated. To better understand valnemulin biotransformation, in this study, metabolites of valnemulinin in in vitro and in vivo rats, chickens, swines, goats, and cows were identified and elucidated using ultraperformance liquid chromatography–quadrupole/time-of-flight hybrid mass spectrometry (UPLC-Q/TOF-MS). As a result, there were totally 7 metabolites of valnemulin identified in vitro and 75, 61, and 74 metabolites detected in in vivo rats, chickens, and swines, respectively, and the majority of metabolites were reported for the first time. The main metabolic pathways of valnemulin were found to be hydroxylation in the mutilin part (the ring system) and the side chain, oxidization on the sulfur of the side chain to form S-oxides, hydrolysis of the amido bond, and acetylization in the amido of the side chain. In addition, hydroxylation in the mutilin part was proposed to be the primary metabolic route. Furthermore, the results revealed that 2β-hydroxyvalnemulin (V1) and 8α-hydroxyvalnemulin (V2) were the major metabolites for rats and swines and S-oxides (V6) in chickens. PMID:25156794

  14. Quantification of short- and medium-chain chlorinated paraffins in environmental samples by gas chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Gao, Wei; Wu, Jing; Wang, Yawei; Jiang, Guibin

    2016-06-24

    Chlorinated paraffins (CPs) are technical products produced and used in bulk for a number of purposes. However, the analysis of CPs is challenging, as they are complex mixtures of compounds and isomers. We herein report the development of an analytical method for the analysis of short-chain CPs (SCCPs) and medium-chain CPs (MCCPs) using quadrupole time-of-flight high-resolution mass spectrometry (GC-NCI-qTOF-HRMS). This method employs gas chromatography with a chemical ionization source working in negative mode. The linear relationship between chlorination and the CP total response factors was applied to quantify the CP content and the congener group distribution patterns. In a single injection, 24 SCCP formula groups and 24 MCCP formula groups were quantified. Extraction of accurate masses using qTOF-HRMS allowed the SCCPs and MCCPs to be distinguished, with interference from other chemicals (e.g., PCBs) being largely avoided. The SCCP and MCCP detection limits were 24-81ng/mL and 27-170ng/mL, respectively. Comparison of the obtained results with analytical results from gas chromatography coupled with electron capture negative ionization low-resolution mass spectrometry (GC-ECNI-LRMS) indicate that the developed technique is a more accurate and convenient method for the analysis of CPs in samples from a range of matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Simultaneous determination of thiamethoxam, clothianidin, and metazachlor residues in soil by ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Valverde, Silvia; Ares, Ana M; Bernal, José Luis; Nozal, María Jesús; Bernal, José

    2017-03-01

    A rapid pioneering method has been developed to simultaneously determine residues of three pesticides (thiamethoxam, clothianidin, and metazachlor) in soil by ultrahigh performance liquid chromatography coupled to a mass spectrometry detector (quadrupole time-of-flight). An efficient extraction procedure (90-105% average analyte recoveries) has also been proposed, involving solid-liquid extraction by a mixture of water and methanol (60:40, v/v), centrifugation, and concentration. A chromatographic analysis of the compounds was achieved in 5.5 min by means of a core-shell technology based column (Kinetex ® EVO C 18 , 50 × 2.1 mm, 1.7 μm, 100 Å). The mobile phase (0.3 mL/min, gradient elution mode) consisted of 0.1% v/v formic acid in water and 0.1% v/v formic acid in acetonitrile. The method was fully validated in terms of selectivity, detection and quantification limits, matrix effect, linearity, trueness, and precision. Low limits of detection and quantification were obtained, ranging from 0.2 to 3.0 μg/kg, which are similar to those published in previous studies, while the absence of a significant matrix effect allowed quantification of the pesticides with standard calibration curves. The proposed method was applied for an analysis of pesticides in several soil samples from experimental fields dedicated to oilseed rape cultivars. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Introduction of a 20 kHz Nd:YVO4 laser into a hybrid quadrupole time-of-flight mass spectrometer for MALDI-MS imaging.

    Science.gov (United States)

    Trim, Paul J; Djidja, Marie-Claude; Atkinson, Sally J; Oakes, Keith; Cole, Laura M; Anderson, David M G; Hart, Philippa J; Francese, Simona; Clench, Malcolm R

    2010-08-01

    A commercial hybrid quadrupole time-of-flight mass spectrometer has been modified for high-speed matrix-assisted laser desorption ionisation (MALDI) imaging using a short-pulse optical technology Nd:YVO(4) laser. The laser operating in frequency-tripled mode (lambda = 355 nm) is capable of delivering 1.5-ns pulses of energy at up to 8 microJ at 5-10 kHz and 3 microJ at 20 kHz. Experiments to improve beam homogeneity and reduce laser speckle by mechanical vibration of the fibre-optic laser delivery system are reported along with data from trial and tissue imaging experiments using the modified instrument. The laser appeared to yield best results for MALDI-MS imaging experiments when operating at repetition rates 5-10 kHz. Combining this with raster imaging allowed images of rat brain sections to be recorded in 37 min. Similarly, images of the distribution of peptides in "on-tissue" digest experiments from tumour tissues were recorded in 1 h and 30 min rather than the 8-h acquisition time previously used. A brief investigation of targeted protein analysis/imaging by multiple reaction monitoring experiments "on-tissue" is reported. A total of 26 transitions were recorded over a 3-s cycle time and images of abundant proteins were successfully recorded.

  17. Simultaneous quantitative determination of 11 sesquiterpene lactones in Jerusalem artichoke (Helianthus tuberosus L.) leaves by ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Yuan, Xiaoyan; Yang, Qianxu

    2017-04-01

    A method of ultra high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry was developed for the simultaneous quantification of 11 sesquiterpene lactones in 11 Jerusalem artichoke leaf samples harvested in a number of areas at different periods. The optimal chromatographic conditions were achieved on a ZORBAX Eclipse Plus C 18 column (3.0 × 150 mm, 1.8 μm) with linear gradient elution of methanol and water in 8 min. Quantitative analysis was carried out under selective ion monitoring mode. All of the sesquiterpene lactones showed good linearity (R 2 ≥ 0.9949), repeatability (relative standard deviations Jerusalem artichoke leaf samples from different areas. Among them, the content of sesquiterpene lactones in the sample collected from Dalian, Liaoning province was the highest and the early flowering period was considered to be the optimal harvest time. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Characterization and classification of seven citrus herbs by liquid chromatography-quadrupole time-of-flight mass spectrometry and genetic algorithm optimized support vector machines.

    Science.gov (United States)

    Duan, Li; Guo, Long; Liu, Ke; Liu, E-Hu; Li, Ping

    2014-04-25

    Citrus herbs have been widely used in traditional medicine and cuisine in China and other countries since the ancient time. However, the authentication and quality control of Citrus herbs has always been a challenging task due to their similar morphological characteristics and the diversity of the multi-components existed in the complicated matrix. In the present investigation, we developed a novel strategy to characterize and classify seven Citrus herbs based on chromatographic analysis and chemometric methods. Firstly, the chemical constituents in seven Citrus herbs were globally characterized by liquid chromatography combined with quadrupole time-of-flight mass spectrometry (LC-QTOF-MS). Based on their retention time, UV spectra and MS fragmentation behavior, a total of 75 compounds were identified or tentatively characterized in these herbal medicines. Secondly, a segmental monitoring method based on LC-variable wavelength detection was developed for simultaneous quantification of ten marker compounds in these Citrus herbs. Thirdly, based on the contents of the ten analytes, genetic algorithm optimized support vector machines (GA-SVM) was employed to differentiate and classify the 64 samples covering these seven herbs. The obtained classifier showed good prediction performance and the overall prediction accuracy reached 96.88%. The proposed strategy is expected to provide new insight for authentication and quality control of traditional herbs. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Identification of metabolites of vindoline in rats using ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Yuqian; Sun, Yupeng; Mu, Xiyan; Yuan, Lin; Wang, Qiao; Zhang, Lantong

    2017-08-15

    Vindoline (VDL) is an indole alkaloid, possessing hypoglycemic and vasodilator effects, and it is also the prodrug of many vinca alkaloids. In this paper, we analyzed in vivo (including plasma, urine, bile and faeces) and in vitro metabolic profile of VDL in rat with ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS/MS). The chromatographic separation was performed on a C 18 column with a mobile phase consisted of 3mM ammonium acetate buffer and acetonitrile at a flow rate of 300μL/min. The mass spectral analysis was conducted in a positive electrospray ionization mode, and on-line data acquisition method multiple mass defect filter (MMDF) combined with dynamic background subtraction (DBS) were used in the biological samples analysis to trace all the potential metabolites of VDL. Twenty-five metabolites of VDL were detected by comparing with the blank sample, of which there were 2 sulfate conjugates. These data suggested that the biotransformation of VDL was deacetylation, oxidation, deoxidization, methylation, dealkylation and sulfate conjugation. This study provides useful information for further study of the pharmacology and mechanism of VDL, meanwhile, the research method can be widely applied to speculate structural features of the metabolites of other vinca alkaloids. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Metabolic Profiling of Hoodia, Chamomile, Terminalia Species and Evaluation of Commercial Preparations Using Ultrahigh-Performance Liquid Chromatography Quadrupole-Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Avula, Bharathi; Wang, Yan-Hong; Isaac, Giorgis; Yuk, Jimmy; Wrona, Mark; Yu, Kate; Khan, Ikhlas A

    2017-11-01

    Ultrahigh-performance liquid chromatography quadrupole-time-of-flight mass spectrometry (UHPLC-QToF-MS) profiling was used for the identification of marker compounds and generation of metabolic patterns that could be interrogated using chemometric modeling software. UHPLC-QToF-MS was used to generate comprehensive fingerprints of three botanicals ( Hoodia, Terminalia , and chamomile), each having different classes of compounds. Detection of a broad range of ions was carried out in full scan mode in both positive and negative modes over the range m/z 100-1700 using high-resolution mass spectrometry. Multivariate statistical analysis was used to extract relevant chemical information from the data to easily differentiate between Terminalia species, chamomile varieties, and quality control of Hoodia products. Using nontargeted analysis, identification of 37 compounds contributed to the differences between Terminalia species, 26 flavonoids were identified to show the differences between German and Roman chamomile, and 43 pregnane glycosides were identified from Hoodia gordonii samples. The UHPLC-QToF-MS-based chemical fingerprinting with principal component analysis was able to correctly distinguish botanicals and their commercial products. This work can be used as a basis to assure the quality of botanicals and commercial products. Georg Thieme Verlag KG Stuttgart · New York.

  1. Metabolomic approaches for orange origin discrimination by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Díaz, Ramon; Pozo, Oscar J; Sancho, Juan V; Hernández, Félix

    2014-08-15

    In this work, hybrid quadrupole time-of-flight mass spectrometer (QTOF MS) coupled to ultra high performance liquid chromatography (UHPLC) has been used for biomarkers identification for correct authentication of Valencia (Spain) oranges. Differentiation from foreign Argentinean, Brazilian and South African oranges has been carried out using XCMS application and multivariate analysis to UHPLC-(Q)TOF MS data acquired in both, positive and negative ionisation modes. Several markers have been found and corroborated by analysing two seasons samples. A seasonal independent marker was found and its structure elucidated using accurate mass data and MS(E) fragmentation spectrum information. Empirical formula was searched in Reaxys database applying sub-structure filtering from the fragments obtained. Three possible structures were found and citrusin D, a compound present in sweet oranges, has been identified as the most plausible as it fits better with the product ion scan performed for this compound. As a result of data obtained in this work, citrusin D is suggested as a potential marker to distinguish the geographic origin of oranges. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Metabolomic study of corticosterone-induced cytotoxicity in PC12 cells by ultra performance liquid chromatography-quadrupole/time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Hongye; Zheng, Hua; Zhao, Gan; Tang, Chaoling; Lu, Shiyin; Cheng, Bang; Wu, Fang; Wei, Jinbin; Liang, Yonghong; Ruan, Junxiang; Song, Hui; Su, Zhiheng

    2016-03-01

    Glucocorticoids (GCs) have been proved to be an important pathogenic factor of some neuropsychiatric disorders. Usually, a classical injury model based on corticosterone-induced cytotoxicity of differentiated rat pheochromocytoma (PC12) cells was used to stimulate the state of GC damage of hippocampal neurons and investigate its potential mechanisms involved. However, up to now, the mechanism of corticosterone-induced cytotoxicity in PC12 cells was still looking forward to further elucidation. In this work, the metabolomic study of the biochemical changes caused by corticosterone-induced cytotoxicity in differentiated PC12 cells with different corticosterone concentrations was performed for the first time, using the ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q/TOF MS). Partial least squares-discriminate analysis (PLS-DA) indicated that metabolic profiles of different corticosterone treatment groups deviated from the control group. A total of fifteen metabolites were characterized as potential biomarkers involved in corticosterone-induced cytotoxicity, which were corresponding to the dysfunctions of five pathways including glycerophospholipid metabolism, sphingolipid metabolism, oxidation of fatty acids, glycerolipid metabolism and sterol lipid metabolism. This study indicated that the rapid and holistic cell metabolomics approach might be a powerful tool to further study the pathogenesis mechanism of corticosterone-induced cytotoxicity in PC12 cells.

  3. Rare earth elements determined in Antarctic ice by inductively coupled plasma-Time of flight, quadrupole and sector field-mass spectrometry: An inter-comparison study

    International Nuclear Information System (INIS)

    Dick, D.; Wegner, A.; Gabrielli, P.; Ruth, U.; Barbante, C.; Kriews, M.

    2008-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is a suitable tool for multi-element analysis at low concentration levels. Rare earth element (REE) determinations in standard reference materials and small volumes of molten ice core samples from Antarctica have been performed with an ICP-time of flight-MS (ICP-TOF-MS) system. Recovery rates for REE in e.g. SPS-SW1 amounted to ∼103%, and the relative standard deviations were 3.4% for replicate analysis at REE concentrations in the lower ng L -1 range. Analyses of REE concentrations in Antarctic ice core samples showed that the ICP-TOF-MS technique meets the demands of restricted sample mass. The data obtained are in good agreement with ICP-Quadrupole-MS (ICP-Q-MS) and ICP-Sector Field-MS (ICP-SF-MS) results. The ICP-TOF-MS system determines accurately and precisely REE concentrations exceeding 5 ng L -1 while between 0.5 and 5 ng L -1 accuracy and precision are element dependent

  4. A Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry (LC-Q-TOF MS) Study for Analyzing 35 Corticosteroid Compounds: Elucidation of MS/MS Fragmentation Pathways

    Energy Technology Data Exchange (ETDEWEB)

    Noh, Eunyoung; Yoon, Chang-Yong; Lee, Ji Hyun; Baek, Sun-Young; Do, Jung-Ah [Ministry of Food and Drug Safety, Cheongju (Korea, Republic of); Lee, Jung-min; Oh, Han Bin [Sogang University, Seoul (Korea, Republic of)

    2016-07-15

    Corticosteroids have been often found to be added to a dietary supplement for the purpose of illegally improving the effect of their products. Thus, it is imperative to develop or improve a method that enables one to rapidly and reliably analyze corticosteroids in health or dietary supplements, for the safety management purpose. In the present study, results from liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS) experiments for the selected 35 corticosteroid compounds are presented, which can be useful for the qualitative screening of corticosteroids in health or dietary supplements. Specifically, retention times, accurate mass data of the protonated steroids, m/z values of major fragment ions are given for the 35 corticosteroids. Further, fragmentation pathways for the selected steroids are also suggested. Based on the suggested fragmentation pathways, it was shown that an unknown steroid compound can be readily identified using the knowledge of a group of unique and specific common skeletal fragments. The high selectivity and sensitivity of the LC-Q-TOF-MS/MS results combined with the knowledge of the fragmentation pathways can offer a new opportunity for rapid and accurate screening of corticosteroids, thus preventing health-related incidents involving adulterated products and clamping down on illegally circulated health products.

  5. Liquid chromatography/quadrupole-time-of-flight mass spectrometry with metabolic profiling of human urine as a tool for environmental analysis of dextromethorphan.

    Science.gov (United States)

    Thurman, E Michael; Ferrer, Imma

    2012-10-12

    We use the combination of liquid chromatography/quadrupole-time-of-flight mass spectrometry (LC/Q-TOF-MS) and urine metabolic profiling to find and identify the metabolites of dextromethorphan, a common over-the-counter (OTC) cough suppressant. Next, we use the combination of ion masses, their MS/MS fragmentation, and retention times to determine dextromethorphan and its metabolites in surface water impacted by wastewater. Prior to this study, neither dextromethorphan nor its metabolites have been reported in surface water; in spite of its common use in over 100 various OTC medications. We found that the concentration of the dextrorphan metabolite in surface water greatly exceeded the parent compound by factors of 5-10 times, which reflects the urine profile, where parent compound is approximately <2% of the total excreted drug based on ion intensities. Urine profiling also indicated that glucuronide metabolites are major phase 2 products (92% of the total) in urine and then are completely hydrolyzed in wastewater to dextrorphan and N-demethyldextrorphan, which are phase 1 metabolites-a "kind of reversal" of human metabolism. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Tentative Structural Assignment of a Glucuronide Metabolite of Methyltestosterone in Tilapia Bile by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Nishshanka, Upul; Chu, Pak-Sin; Evans, Eric; Reimschuessel, Renate; Hasbrouck, Nicholas; Amarasinghe, Kande; Jayasuriya, Hiranthi

    2015-06-24

    Methyltestosterone (MT), a strong androgenic steroid, is not approved for use in fish aquaculture in the United States. It is used in the U.S. under an investigational new animal drug exemption (INAD) only during the early life stages of fish. There is a possibility that farmers feed fish with MT to enhance production for economic gains. Therefore, there is a need to develop methods for the detection of MT and its metabolite residues in fish tissue for monitoring purposes. Previously, our laboratory developed a liquid chromatography-quadrupole time-of-flight (LC-QTOF) method for characterization of 17-O-glucuronide metabolite (MT-glu) in bile of tilapia dosed with MT. The system used was an Agilent 6530 Q-TOF equipped with electrospray jet stream technology, operating in positive ion mode. Retrospective analysis of the data generated in that experiment by a feature-finding algorithm, combined with a search against an in-house library of possible MT-metabolites, resulted in the discovery of a major glucuronide metabolite of MT in the bile extracts. Preliminary data indicate it to be a glucuronide of a hydroxylated MT (OHMT-glu) which persists in tilapia bile for at least 2 weeks after dosing. We present the tentative structural assignment of the OHMT-glu in tilapia bile and time course of development. This glucuronide can serve as a marker to monitor illegal use of MT in tilapia culture.

  7. Nontarget analysis of polar contaminants in freshwater sediments influenced by pharmaceutical industry using ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Terzic, Senka; Ahel, Marijan

    2011-01-01

    A comprehensive analytical procedure for a reliable identification of nontarget polar contaminants in aquatic sediments was developed, based on the application of ultra-high-pressure liquid chromatography (UHPLC) coupled to hybrid quadrupole time-of-flight mass spectrometry (QTOFMS). The procedure was applied for the analysis of freshwater sediment that was highly impacted by wastewater discharges from the pharmaceutical industry. A number of different contaminants were successfully identified owing to the high mass accuracy of the QTOFMS system, used in combination with high chromatographic resolution of UHPLC. The major compounds, identified in investigated sediment, included a series of polypropylene glycols (n = 3-16), alkylbenzene sulfonate and benzalkonium surfactants as well as a number of various pharmaceuticals (chlorthalidone, warfarin, terbinafine, torsemide, zolpidem and macrolide antibiotics). The particular advantage of the applied technique is its capability to detect less known pharmaceutical intermediates and/or transformation products, which have not been previously reported in freshwater sediments. - Research highlights: → UHPLC-QTOFMS coupling was applied for nontarget analysis of polar contaminants. → Wide spectrum of polar contaminants was identified in polluted sediments. → Pharmaceuticals and their intermediates were present in high concentrations. - Comprehensive analysis of freshwater sediments by UPLC/QTOF indicated importance of pharmaceutically-derived polar contaminants.

  8. Nontarget analysis of polar contaminants in freshwater sediments influenced by pharmaceutical industry using ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Terzic, Senka, E-mail: terzic@irb.h [Division of Marine and Environmental Research, Rudjer Boskovic Institute, 10000 Zagreb (Croatia); Ahel, Marijan [Division of Marine and Environmental Research, Rudjer Boskovic Institute, 10000 Zagreb (Croatia)

    2011-02-15

    A comprehensive analytical procedure for a reliable identification of nontarget polar contaminants in aquatic sediments was developed, based on the application of ultra-high-pressure liquid chromatography (UHPLC) coupled to hybrid quadrupole time-of-flight mass spectrometry (QTOFMS). The procedure was applied for the analysis of freshwater sediment that was highly impacted by wastewater discharges from the pharmaceutical industry. A number of different contaminants were successfully identified owing to the high mass accuracy of the QTOFMS system, used in combination with high chromatographic resolution of UHPLC. The major compounds, identified in investigated sediment, included a series of polypropylene glycols (n = 3-16), alkylbenzene sulfonate and benzalkonium surfactants as well as a number of various pharmaceuticals (chlorthalidone, warfarin, terbinafine, torsemide, zolpidem and macrolide antibiotics). The particular advantage of the applied technique is its capability to detect less known pharmaceutical intermediates and/or transformation products, which have not been previously reported in freshwater sediments. - Research highlights: UHPLC-QTOFMS coupling was applied for nontarget analysis of polar contaminants. Wide spectrum of polar contaminants was identified in polluted sediments. Pharmaceuticals and their intermediates were present in high concentrations. - Comprehensive analysis of freshwater sediments by UPLC/QTOF indicated importance of pharmaceutically-derived polar contaminants.

  9. Distribution patterns of flavonoids from three Momordica species by ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry: a metabolomic profiling approach

    Directory of Open Access Journals (Sweden)

    Ntakadzeni Edwin Madala

    Full Text Available ABSTRACT Plants from the Momordica genus, Curcubitaceae, are used for several purposes, especially for their nutritional and medicinal properties. Commonly known as bitter gourds, melon and cucumber, these plants are characterized by a bitter taste owing to the large content of cucurbitacin compounds. However, several reports have shown an undisputed correlation between the therapeutic activities and polyphenolic flavonoid content. Using ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry in combination with multivariate data models such as principal component analysis and hierarchical cluster analysis, three Momordica species (M. foetida Schumach., M. charantia L. and M. balsamina L. were chemo-taxonomically grouped based on their flavonoid content. Using a conventional mass spectrometric-based approach, thirteen flavonoids were tentatively identified and the three species were found to contain different isomers of the quercetin-, kaempferol- and isorhamnetin-O-glycosides. Our results indicate that Momordica species are overall very rich sources of flavonoids but do contain different forms thereof. Furthermore, to the best of our knowledge, this is a first report on the flavonoid content of M. balsamina L.

  10. Development and Application of an MSALL-Based Approach for the Quantitative Analysis of Linear Polyethylene Glycols in Rat Plasma by Liquid Chromatography Triple-Quadrupole/Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Zhou, Xiaotong; Meng, Xiangjun; Cheng, Longmei; Su, Chong; Sun, Yantong; Sun, Lingxia; Tang, Zhaohui; Fawcett, John Paul; Yang, Yan; Gu, Jingkai

    2017-05-16

    Polyethylene glycols (PEGs) are synthetic polymers composed of repeating ethylene oxide subunits. They display excellent biocompatibility and are widely used as pharmaceutical excipients. To fully understand the biological fate of PEGs requires accurate and sensitive analytical methods for their quantitation. Application of conventional liquid chromatography-tandem mass spectrometry (LC-MS/MS) is difficult because PEGs have polydisperse molecular weights (MWs) and tend to produce multicharged ions in-source resulting in innumerable precursor ions. As a result, multiple reaction monitoring (MRM) fails to scan all ion pairs so that information on the fate of unselected ions is missed. This Article addresses this problem by application of liquid chromatography-triple-quadrupole/time-of-flight mass spectrometry (LC-Q-TOF MS) based on the MS ALL technique. This technique performs information-independent acquisition by allowing all PEG precursor ions to enter the collision cell (Q2). In-quadrupole collision-induced dissociation (CID) in Q2 then effectively generates several fragments from all PEGs due to the high collision energy (CE). A particular PEG product ion (m/z 133.08592) was found to be common to all linear PEGs and allowed their total quantitation in rat plasma with high sensitivity, excellent linearity and reproducibility. Assay validation showed the method was linear for all linear PEGs over the concentration range 0.05-5.0 μg/mL. The assay was successfully applied to the pharmacokinetic study in rat involving intravenous administration of linear PEG 600, PEG 4000, and PEG 20000. It is anticipated the method will have wide ranging applications and stimulate the development of assays for other pharmaceutical polymers in the future.

  11. Resveratrol Metabolism in a Non-Human Primate, the Grey Mouse Lemur (Microcebus murinus), Using Ultra-High-Performance Liquid Chromatography–Quadrupole Time of Flight

    Science.gov (United States)

    Menet, Marie-Claude; Marchal, Julia; Dal-Pan, Alexandre; Taghi, Méryam; Nivet-Antoine, Valérie; Dargère, Delphine; Laprévote, Olivier; Beaudeux, Jean-Louis; Aujard, Fabienne; Epelbaum, Jacques; Cottart, Charles-Henry

    2014-01-01

    The grey mouse lemur (Microcebus murinus) is a non-human primate used to study the ageing process. Resveratrol is a polyphenol that may increase lifespan by delaying age-associated pathologies. However, no information about resveratrol absorption and metabolism is available for this primate. Resveratrol and its metabolites were qualitatively and quantitatively analyzed in male mouse-lemur plasma (after 200 mg.kg−1 of oral resveratrol) by ultra-high performance liquid chromatography (UHPLC), coupled to a quadrupole-time-of-flight (Q-TOF) mass spectrometer used in full-scan mode. Data analyses showed, in MSE mode, an ion common to resveratrol and all its metabolites: m/z 227.072, and an ion common to dihydro-resveratrol metabolites: m/z 229.08. A semi-targeted study enabled us to identify six hydrophilic resveratrol metabolites (one diglucurono-conjugated, two monoglucurono-conjugated, one monosulfo-conjugated and two both sulfo- and glucurono-conjugated derivatives) and three hydrophilic metabolites of dihydro-resveratrol (one monoglucurono-conjugated, one monosulfo-conjugated, and one both sulfo- and glucurono-conjugated derivatives). The presence of such metabolites has been already detected in the mouse, rat, pig, and humans. Free resveratrol was measurable for several hours in mouse-lemur plasma, and its two main metabolites were trans-resveratrol-3-O-glucuronide and trans-resveratrol-3-sulfate. Free dihydro-resveratrol was not measurable whatever the time of plasma collection, while its hydrophilic metabolites were present at 24 h after intake. These data will help us interpret the effect of resveratrol in mouse lemurs and provide further information on the inter-species characteristics of resveratrol metabolism. PMID:24663435

  12. Unbiased metabolite profiling by liquid chromatography-quadrupole time-of-flight mass spectrometry and multivariate data analysis for herbal authentication: classification of seven Lonicera species flower buds.

    Science.gov (United States)

    Gao, Wen; Yang, Hua; Qi, Lian-Wen; Liu, E-Hu; Ren, Mei-Ting; Yan, Yu-Ting; Chen, Jun; Li, Ping

    2012-07-06

    Plant-based medicines become increasingly popular over the world. Authentication of herbal raw materials is important to ensure their safety and efficacy. Some herbs belonging to closely related species but differing in medicinal properties are difficult to be identified because of similar morphological and microscopic characteristics. Chromatographic fingerprinting is an alternative method to distinguish them. Existing approaches do not allow a comprehensive analysis for herbal authentication. We have now developed a strategy consisting of (1) full metabolic profiling of herbal medicines by rapid resolution liquid chromatography (RRLC) combined with quadrupole time-of-flight mass spectrometry (QTOF MS), (2) global analysis of non-targeted compounds by molecular feature extraction algorithm, (3) multivariate statistical analysis for classification and prediction, and (4) marker compounds characterization. This approach has provided a fast and unbiased comparative multivariate analysis of the metabolite composition of 33-batch samples covering seven Lonicera species. Individual metabolic profiles are performed at the level of molecular fragments without prior structural assignment. In the entire set, the obtained classifier for seven Lonicera species flower buds showed good prediction performance and a total of 82 statistically different components were rapidly obtained by the strategy. The elemental compositions of discriminative metabolites were characterized by the accurate mass measurement of the pseudomolecular ions and their chemical types were assigned by the MS/MS spectra. The high-resolution, comprehensive and unbiased strategy for metabolite data analysis presented here is powerful and opens the new direction of authentication in herbal analysis. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Development and validation of an ultra-performance liquid chromatography quadrupole time of flight mass spectrometry method for rapid quantification of free amino acids in human urine.

    Science.gov (United States)

    Joyce, Richard; Kuziene, Viktorija; Zou, Xin; Wang, Xueting; Pullen, Frank; Loo, Ruey Leng

    2016-01-01

    An ultra-performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-qTOF-MS) method using hydrophilic interaction liquid chromatography was developed and validated for simultaneous quantification of 18 free amino acids in urine with a total acquisition time including the column re-equilibration of less than 18 min per sample. This method involves simple sample preparation steps which consisted of 15 times dilution with acetonitrile to give a final composition of 25 % aqueous and 75 % acetonitrile without the need of any derivatization. The dynamic range for our calibration curve is approximately two orders of magnitude (120-fold from the lowest calibration curve point) with good linearity (r (2) ≥ 0.995 for all amino acids). Good separation of all amino acids as well as good intra- and inter-day accuracy (amino acids in the prepared urine samples was found to be stable for 72 h at 4 °C, after one freeze thaw cycle and for up to 4 weeks at -80 °C. We have applied this method to quantify the content of 18 free amino acids in 646 urine samples from a dietary intervention study. We were able to quantify all 18 free amino acids in these urine samples, if they were present at a level above the LOD. We found our method to be reproducible (accuracy and precision were typically <10 % for QCL, QCM and QCH) and the relatively high sample throughput nature of this method potentially makes it a suitable alternative for the analysis of urine samples in clinical setting.

  14. Comprehensive Analysis of Tiamulin Metabolites in Various Species of Farm Animals Using Ultra-High-Performance Liquid Chromatography Coupled to Quadrupole/Time-of-Flight.

    Science.gov (United States)

    Sun, Feifei; Yang, Shupeng; Zhang, Huiyan; Zhou, Jinhui; Li, Yi; Zhang, Jinzhen; Jin, Yue; Wang, Zhanhui; Li, Yanshen; Shen, Jianzhong; Zhang, Suxia; Cao, Xingyuan

    2017-01-11

    Tiamulin is an antimicrobial widely used in veterinary practice to treat dysentery and pneumonia in pigs and poultry. However, knowledge about the metabolism of tiamulin is very limited in farm animals. To better understand the biotransformation of tiamulin, in the present study, in vitro and in vivo metabolites of tiamulin in rats, chickens, swine, goats, and cows were identified and elucidated using ultra-high performance liquid chromatography coupled to quadrupole/time-of-flight. As a result, a total of 26 metabolites of tiamulin, identified in vitro and in vivo, and majority of metabolites were revealed for the first time. In all farm animals, tiamulin undergoes phase I metabolic routes of hydroxylation in the mutilin part (the ring system), S-oxidation and N-deethylation on side chain, and no phase II metabolite was detected. Among these, 2β- and 8α-hydroxylation and N-deethylation were the main metabolic pathways of tiamulin in farm animals. In addition, we have put forward that 8a-hydroxy-tiamulin and 8a-hydroxy-N-deethyl-tiamulin could be hydroxylated into 8a-hydroxy-mutilin, the marker residue of tiamulin in swine. Furthermore, a significant interspecies difference was observed on the metabolism of tiamulin among various farm animals. The possible marker residues for tiamulin in swine were 8α-hydroxy-tiamulin, N-deethyl-tiamulin, and 8α-hydroxy-N-deethyl-tiamulin, which were consistent with the hypothesis proposed by the European Agency for the Evaluation of Medicinal Products. However, results in present study indicated that three metabolites (2β-hydroxy-tiamulin, N-deethyl-tiamulin, and 2β-hydroxy-N-deethyl-tiamulin) of tiamulin in chickens had larger yields, which implied that 2β-hydroxy-mutilin or N-deethyl-tiamulin was more likely to be regarded as the potential marker residue of tiamulin in chickens.

  15. Antioxidant activity and identification of bioactive compounds from leaves of Anthocephalus cadamba by ultra-performance liquid chromatography/electrospray ionization quadrupole time of flight mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Madhu Chandel; Upendra Sharma; Neeraj Kumar; Bikram Singh; Satwinderjeet Kaur

    2012-01-01

    Objective: To evaluate the antioxidant potential of different extract/fractions of Anthocephalus cadamba (A. cadamba) (Roxb.) Miq. (Rubiaceae) and study the tentative identification of their active constituents. Methods: The extract/fractions were screened for antioxidant activity using various in vitro assays viz. DPPH assay, ABTS assay, superoxide anion radical scavenging assay, reducing power assay and plasmid DNA nicking assay. Total phenolic content of extract/fractions was determined by colorimetric method. An ultra-performance LC-electrospray-quadrupole-time of flight mass spectrometry method was used to analyse the active constituents of extract/fractions of A. cadamba. Results: The ethyl acetate fraction was found to be most active fraction in all the assays as compared to other extract/fractions. The IC50 value of ethyl acetate fraction (ETAC fraction) was 21.24 μg/mL, 1.12 μg/mL, 9.68 μg/mL and 57.81 μg/mL in DPPH assay, ABTS assay, reducing power assay and superoxide scavenging assay respectively. All the extract/fractions also showed the potential to protect the plasmid DNA (pBR322) against the attack of hydroxyl radicals generated by Fenton’s reagent. The bioactive compounds were identified by UPLC-ESI-QTOF-MS, by comparing the mass and λmax with literature values. Conclusions: The potential of the extract/fractions to scavenge different free radicals in different systems indicated that they may be useful therapeutic agents for treating radical-related pathologic damage.

  16. Rapid Quantification and Quantitation of Alkaloids in Xinjiang Fritillaria by Ultra Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Aziz Mohammat

    2017-05-01

    Full Text Available The Fritillaria genus, including different kinds of medicinal and edible plants belonging to the Liliaceae family which have the function of treating and relieving a cough and eliminating phlegm, is widely planted in Xinjiang (China. There are few comprehensive studies reporting on the characterization of the chemical constituents of Fritillaria from Xinjiang, and to date, no work describing the quantitative differences between the components in Fritillaria from Xinjiang and related species. The purpose of this study was to develop qualitative and quantitative analytical methods by Ultra Performance Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry (UPLC-QTOF-MS for the rapid quantification and quantitation of alkaloids in wild and cultivated Xinjiang Fritillaria, which could be used in the quality control of medicine based on this natural herb. Using the UPLC-QTOF-MS method, the chemical constituents of Xinjiang Fritillaria were identified by fragmentation information and retention behavior, and were compared to reference standards. Furthermore, a quantitative comparision of four major alkaloids in wild and cultivated Xinjiang Fritillaria was conducted by determining the content of Sipeimine-3β-d-glucoside, Sipeimine, Peimisine, and Yibeinoside A, respectively. A total of 89 characteristic peaks, including more than 40 alkaloids, were identified in the chromatographic results of Fritillaria. Four main alkaloids were quantified by using a validated method based on UPLC-QTOF-MS. The relative contents of Sipeimine-3β-d-glucoside, Sipeimine, Peimisine, and Yibeinoside A varied from 0.0013%~0.1357%, 0.0066%~0.1218%, 0.0033%~0.0437%, and 0.0019%~0.1398%, respectively. A rough separation of wild and cultivated Fritillaria could be achieved by the cluster analysis method.

  17. Strategy for Comprehensive Profiling and Identification of Acidic Glycosphingolipids Using Ultra-High-Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Hu, Ting; Jia, Zhixin; Zhang, Jin-Lan

    2017-07-18

    Acidic glycosphingolipids (AGSLs), which mainly consist of ganglioside and sulfatide moieties, are highly concentrated in the central nervous system. Comprehensive profiling of AGSLs has historically been challenging because of their high complexity and the lack of standards. In this study, a novel strategy was developed to comprehensively profile AGSLs using ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Ganglioside isomers with different glycan chains such as GD1a/GD1b were completely separated on a C18 column for the first time to our knowledge, facilitated by the addition of formic acid in the mobile phase. A mathematical model was established to predict the retention times (RTs) of all theoretically possible AGSLs on the basis of the good logarithmic relationship between the ceramide carbon numbers of the AGSLs in the reference material and their RTs. A data set was created of 571 theoretically possible AGSLs, including the ceramide carbon numbers, RTs, and high-resolution quasi-molecular ions. A novel fast identification strategy was established for global AGSL profiling by comparing the high-resolution quasi-molecular ions and RTs of the tested peaks to those in the data set of 571 AGSLs. Using this strategy, 199 AGSL candidates were identified in rat brain tissue. MS/MS fragments were further collected for these 199 candidates to confirm their identity as AGSLs. This novel strategy was employed to profile AGSLs in brain tissue samples from control rats and model rats with bilateral common carotid artery (2-VO) cerebral ischemia. Forty AGSLs were significantly different between the control and model groups, and these differences were further interpreted.

  18. Atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for simultaneous determination of fifteen organochlorine pesticides in soil and water.

    Science.gov (United States)

    Cheng, Zhipeng; Dong, Fengshou; Xu, Jun; Liu, Xingang; Wu, Xiaohu; Chen, Zenglong; Pan, Xinglu; Zheng, Yongquan

    2016-02-26

    In this study, the application of atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry (APGC-QTOF-MS) has been investigated for simultaneous determination of fifteen organochlorine pesticides in soil and water. Soft ionization of atmospheric pressure gas chromatography was evaluated by comparing with traditional more energetic electron impact ionization (EI). APGC-QTOF-MS showed a sensitivity enhancement by approximately 7-305 times. The QuEChERs (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was used to pretreat the soil samples and solid phase extraction (SPE) cleanup was used for water samples. Precision, accuracy and stability experiments were undertaken to evaluate the feasibility of the method. The results showed that the mean recoveries for all the pesticides from the soil samples were 70.3-118.9% with 0.4-18.3% intra-day relative standard deviations (RSD) and 1.0-15.6% inter-day RSD at 10, 50 and 500 μg/L levels, while the mean recoveries of water samples were 70.0-118.0% with 1.1-17.8% intra-day RSD and 0.5-12.2% inter-day RSD at 0.1, 0.5 and 1.0 μg/L levels. Excellent linearity (0.9931 ≦ r(2)≤ 0.9999) was obtained for each pesticides in the soil and water matrix calibration curves within the range of 0.01-1.0mg/L. The limits of detection (LOD) for each of the 15 pesticides was less than 3.00 μg/L, while the limit of quantification (LOQ) was less than 9.99 μg/L in soil and water. Furthermore, the developed method was successfully applied to monitor the targeted pesticides in real soil and water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Rapid resolution liquid chromatography coupled with quadrupole time-of-flight mass spectrometry-based metabolomics approach to study the effects of jieduquyuziyin prescription on systemic lupus erythematosus.

    Science.gov (United States)

    Ding, Xinghong; Hu, Jinbo; Wen, Chengping; Ding, Zhishan; Yao, Li; Fan, Yongsheng

    2014-01-01

    Jieduquyuziyin prescription (JP), a traditional Chinese medicine (TCM) prescription, has been widely used for the clinical treatment of systemic lupus erythematosus (SLE). However, the complex chemical constituents of JP and the multifactorial pathogenesis of SLE make research on the therapeutic mechanism of JP in SLE challenging. In this paper, a serum metabolomics approach based on rapid resolution liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (RRLC-Q-TOF/MS) was employed to acquire the metabolic characteristics of serum samples obtained from mice in the SLE model group, JP-treated group, prednisone acetate (PA)-treated group and control group. The orthogonal partial least squares (OPLS) was applied to recognize metabolic patterns, and an obvious separation of groups was obtained. Thirteen metabolites, namely, phosphatidylethanolamine (PE 20:3), hepoxilin B3, lyso- phosphatidylethanolamine (lyso-PE 22:6), 12S-hydroxypentaenoic acid (12S-HEPE), traumatic acid, serotonin, platelet-activating factor (PAF), phosphatidylcholine (PC 20:5),eicosapentaenoic acid (EPA), 12(S)-hydroxyei- cosatetraenoic acid (12S-HETE), 14-hydroxy docosahexaenoic acid (14-HDOHE), lyso-phosphatidylcholine (lyso-PC 20:4), and indole acetaldehyde, were identified and characterized as differential metabolites involved in the pathogenesis of SLE. After treatment with JP, the relative content of 12(S)-HETE, PAF, 12(S)-HEPE, EPA, PE (20:3), Lyso-PE(22:6), and 14-HDOHE were effectively regulated, which suggested that the therapeutic effects of JP on SLE may involve regulating disturbances to the metabolism of unsaturated fatty acid, tryptophan and phospholipid. This research also demonstrated that metabolomics is a powerful tool for researching complex disease mechanisms and evaluating the mechanism of action of TCM.

  20. Suspected-target pesticide screening using gas chromatography-quadrupole time-of-flight mass spectrometry with high resolution deconvolution and retention index/mass spectrum library.

    Science.gov (United States)

    Zhang, Fang; Wang, Haoyang; Zhang, Li; Zhang, Jing; Fan, Ruojing; Yu, Chongtian; Wang, Wenwen; Guo, Yinlong

    2014-10-01

    A strategy for suspected-target screening of pesticide residues in complicated matrices was exploited using gas chromatography in combination with hybrid quadrupole time-of-flight mass spectrometry (GC-QTOF MS). The screening workflow followed three key steps of, initial detection, preliminary identification, and final confirmation. The initial detection of components in a matrix was done by a high resolution mass spectrum deconvolution; the preliminary identification of suspected pesticides was based on a special retention index/mass spectrum (RI/MS) library that contained both the first-stage mass spectra (MS(1) spectra) and retention indices; and the final confirmation was accomplished by accurate mass measurements of representative ions with their response ratios from the MS(1) spectra or representative product ions from the second-stage mass spectra (MS(2) spectra). To evaluate the applicability of the workflow in real samples, three matrices of apple, spinach, and scallion, each spiked with 165 test pesticides in a set of concentrations, were selected as the models. The results showed that the use of high-resolution TOF enabled effective extractions of spectra from noisy chromatograms, which was based on a narrow mass window (5 mDa) and suspected-target compounds identified by the similarity match of deconvoluted full mass spectra and filtering of linear RIs. On average, over 74% of pesticides at 50 ng/mL could be identified using deconvolution and the RI/MS library. Over 80% of pesticides at 5 ng/mL or lower concentrations could be confirmed in each matrix using at least two representative ions with their response ratios from the MS(1) spectra. In addition, the application of product ion spectra was capable of confirming suspected pesticides with specificity for some pesticides in complicated matrices. In conclusion, GC-QTOF MS combined with the RI/MS library seems to be one of the most efficient tools for the analysis of suspected-target pesticide residues

  1. Sensitive screening of abused drugs in dried blood samples using ultra-high-performance liquid chromatography-ion booster-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Chepyala, Divyabharathi; Tsai, I-Lin; Liao, Hsiao-Wei; Chen, Guan-Yuan; Chao, Hsi-Chun; Kuo, Ching-Hua

    2017-03-31

    An increased rate of drug abuse is a major social problem worldwide. The dried blood spot (DBS) sampling technique offers many advantages over using urine or whole blood sampling techniques. This study developed a simple and efficient ultra-high-performance liquid chromatography-ion booster-quadrupole time-of-flight mass spectrometry (UHPLC-IB-QTOF-MS) method for the analysis of abused drugs and their metabolites using DBS. Fifty-seven compounds covering the most commonly abused drugs, including amphetamines, opioids, cocaine, benzodiazepines, barbiturates, and many other new and emerging abused drugs, were selected as the target analytes of this study. An 80% acetonitrile solvent with a 5-min extraction by Geno grinder was used for sample extraction. A Poroshell column was used to provide efficient separation, and under optimal conditions, the analytical times were 15 and 5min in positive and negative ionization modes, respectively. Ionization parameters of both electrospray ionization source and ion booster (IB) source containing an extra heated zone were optimized to achieve the best ionization efficiency of the investigated abused drugs. In spite of their structural diversity, most of the abused drugs showed an enhanced mass response with the high temperature ionization from an extra heated zone of IB source. Compared to electrospray ionization, the ion booster (IB) greatly improved the detection sensitivity for 86% of the analytes by 1.5-14-fold and allowed the developed method to detect trace amounts of compounds on the DBS cards. The validation results showed that the coefficients of variation of intra-day and inter-day precision in terms of the signal intensity were lower than 19.65%. The extraction recovery of all analytes was between 67.21 and 115.14%. The limits of detection of all analytes were between 0.2 and 35.7ngmL -1 . The stability study indicated that 7% of compounds showed poor stability (below 50%) on the DBS cards after 6 months of storage at

  2. Use of quadrupole time-of-flight mass spectrometry to determine proposed structures of transformation products of the herbicide bromacil after water chlorination.

    Science.gov (United States)

    Ibáñez, María; Sancho, Juan V; Pozo, Oscar J; Hernández, Félix

    2011-10-30

    The herbicide bromacil has been extensively used in the Spanish Mediterranean region, and although plant protection products containing bromacil have been withdrawn by the European Union, this compound is still frequently detected in surface and ground water of this area. However, the fast and complete disappearance of this compound has been observed in water intended for human consumption, after it has been subjected to chlorination. There is a concern about the possible degradation products formed, since they might be present in drinking water and might be hazardous. In this work, the sensitive full-spectrum acquisition, high resolution and exact mass capabilities of hybrid quadrupole time-of-flight (QTOF) mass spectrometry have allowed the discovery and proposal of structures of transformation products (TPs) of bromacil in water subjected to chlorination. Different ground water samples spiked at 0.5 µg/mL were subjected to the conventional chlorination procedure applied to drinking waters, sampling 2-mL aliquots at different time intervals (1, 10 and 30 min). The corresponding non-spiked water was used as control sample in each experiment. Afterwards, 50 μL of the water was directly injected into an ultra-high-pressure liquid chromatography (UHPLC)/electrospray ionization (ESI)-(Q)TOF system. The QTOF instrument enabled the simultaneous recording of two acquisition functions at different collision energies (MS(E) approach): the low-energy (LE) function, fixed at 4 eV, and the high-energy (HE) function, with a collision energy ramp from 15 to 40 eV. This approach enables the simultaneous acquisition of both parent (deprotonated and protonated molecules) and fragment ions in a single injection. The low mass errors observed for the deprotonated and protonated molecules (detected in LE function) allowed the assignment of a highly probable molecular formula. Fragment ions and neutral losses were investigated in both LE and HE spectra to elucidate the

  3. Trace analysis of total naphthenic acids in aqueous environmental matrices by liquid chromatography/mass spectrometry-quadrupole time of flight mass spectrometry direct injection.

    Science.gov (United States)

    Brunswick, Pamela; Shang, Dayue; van Aggelen, Graham; Hindle, Ralph; Hewitt, L Mark; Frank, Richard A; Haberl, Maxine; Kim, Marcus

    2015-07-31

    A rapid and sensitive liquid chromatography quadrupole time of flight method has been established for the determination of total naphthenic acid concentrations in aqueous samples. This is the first methodology that has been adopted for routine, high resolution, high throughput analysis of total naphthenic acids at trace levels in unprocessed samples. A calibration range from 0.02 to 1.0μgmL(-1) total Merichem naphthenic acids was validated and demonstrated excellent accuracy (97-111% recovery) and precision (1.9% RSD at 0.02μgmL(-1)). Quantitative validation was also demonstrated in a non-commercial oil sands process water (OSPW) acid extractable organics (AEOs) fraction containing a higher percentage of polycarboxylic acid isomers than the Merichem technical mix. The chromatographic method showed good calibration linearity of ≥0.999 RSQ to 0.005μgmL(-1) total naphthenic acids with a precision <3.1% RSD and a calculated detection limit of 0.0004μgmL(-1) employing Merichem technical mix reference material. The method is well suited to monitoring naturally occurring and industrially derived naphthenic acids (and other AEOs) present in surface and ground waters in the vicinity of mining developments. The advantage of the current method is its direct application to unprocessed environmental samples and to examine natural naphthenic acid isomer profiles. It is noted that where the isomer profile of samples differs from that of the reference material, results should be considered semi-quantitative due to the lack of matching isomer content. The fingerprint profile of naphthenic acids is known to be transitory during aging and the present method has the ability to adapt to monitoring of these changes in naphthenic acid content. The method's total ion scan approach allows for data previously collected to be examined retrospectively for specific analyte mass ions of interest. A list of potential naphthenic acid isomers that decrease in response with aging is proposed

  4. 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

  5. Elemental analysis of coal by tandem laser induced breakdown spectroscopy and laser ablation inductively coupled plasma time of flight mass spectrometry

    International Nuclear Information System (INIS)

    Dong, Meirong; Oropeza, Dayana; Chirinos, José; González, Jhanis J.; Lu, Jidong; Mao, Xianglei; Russo, Richard E.

    2015-01-01

    The capabilities and analytical benefits of combined LIBS and LA-ICP-MS were evaluated for the analysis of coal samples. The ablation system consisted of a Nd:YAG laser operated 213 nm. A Czerny-turner spectrograph with ICCD detector and time-of-flight based mass spectrometer were utilized for LIBS and ICP-MS detection, respectively. This tandem approach allows simultaneous determination of major and minor elements (C, Si, Ca, Al, Mg), and trace elements (V, Ba, Pb, U, etc.) in the coal samples. The research focused on calibration strategies, specifically the use of univariate and multivariate data analysis on analytical performance. Partial least square regression (PLSR) was shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The correlation between measurements from these two techniques demonstrated that mass spectral data combined with LIBS emission measurements by PLSR improved the accuracy and precision for quantitative analysis of trace elements in coal. - Highlights: • Tandem LIBS LA-ICP-MS • Simultaneous determination of major and minor elements and trace elements in the coal samples. • Extended Dynamic Range • Correlation between LIBS with LA-ICP-MS demonstrated improved the accuracy and precision for quantitative analysis of coal

  6. Elemental analysis of coal by tandem laser induced breakdown spectroscopy and laser ablation inductively coupled plasma time of flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Meirong [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Oropeza, Dayana [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Chirinos, José [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Escuela de Química, Facultad de Ciencias, Universidad Central de Venezuela, Caracas 1041a (Venezuela, Bolivarian Republic of); González, Jhanis J. [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Lu, Jidong [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Mao, Xianglei [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Russo, Richard E., E-mail: RERusso@lbl.gov [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States)

    2015-07-01

    The capabilities and analytical benefits of combined LIBS and LA-ICP-MS were evaluated for the analysis of coal samples. The ablation system consisted of a Nd:YAG laser operated 213 nm. A Czerny-turner spectrograph with ICCD detector and time-of-flight based mass spectrometer were utilized for LIBS and ICP-MS detection, respectively. This tandem approach allows simultaneous determination of major and minor elements (C, Si, Ca, Al, Mg), and trace elements (V, Ba, Pb, U, etc.) in the coal samples. The research focused on calibration strategies, specifically the use of univariate and multivariate data analysis on analytical performance. Partial least square regression (PLSR) was shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The correlation between measurements from these two techniques demonstrated that mass spectral data combined with LIBS emission measurements by PLSR improved the accuracy and precision for quantitative analysis of trace elements in coal. - Highlights: • Tandem LIBS LA-ICP-MS • Simultaneous determination of major and minor elements and trace elements in the coal samples. • Extended Dynamic Range • Correlation between LIBS with LA-ICP-MS demonstrated improved the accuracy and precision for quantitative analysis of coal.

  7. 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...

  8. Matrix effect in analysis of pesticide residues in fruits and vegetables by high performance liquid chromatography with quadrupole-time of flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    Andoralov A.M.

    2017-03-01

    Full Text Available For modern food safety control are using techniques that allow to determinate a large number of components. So for determination of pesticide residues in fruits and vegetables commonly used methods of gas and liquid chromatography with time-of-flight mass-spectrometric detection. This system allows to carry out quantitative determination several hundreds of pesticides and their identification by the characteristic fragments of the mass spectrum. The main problem when using mass spectrometric detection is a matrix effect, which is caused by the influence of matrix components extracted with pesticides from the sample. In this work, attempts have been made to reduce the influence of the matrix in the analysis of pesticide residues by high performance liquid chromatography with time of flight mass spectrometry (HPLC / TOFMS.

  9. A Tandem-electrostatic-quadrupole for accelerator-based BNCT

    International Nuclear Information System (INIS)

    Kreiner, A.J.; Kwan, J.W.; Burlon, A.A.; Di Paolo, H.; Henestroza, E.; Minsky, D.M.; Valda, A.A.; Debray, M.E.; Somacal, H.

    2007-01-01

    A project to develop a Tandem-electrostatic-quadrupole (TESQ) accelerator for accelerator-based boron neutron capture therapy (AB-BNCT) is described. A folded Tandem, with 1.25 MV terminal voltage, combined with an electrostatic quadrupole (ESQ) chain is being proposed. The project goal is a machine capable of delivering 30 mA of 2.5 MeV protons to be used in conjunction with a neutron production target based on the 7 Li(p, n) 7 Be reaction slightly beyond its resonance at 2.25 MeV. This machine is conceptually shown to be capable of accelerating a 30 mA proton beam to 2.5 MeV. These are the specifications needed to produce sufficiently intense and clean epithermal neutron beams, based on the 7 Li(p, n) 7 Be reaction, to perform BNCT treatment for deep-seated tumors in less than an hour. This electrostatic machine is the technologically simplest and cheapest solution for optimized AB-BNCT

  10. Qualitative and quantitative characterization of secondary metabolites and carbohydrates in Bai-Hu-Tang using ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and ultraperformance liquid chromatography coupled with photodiode array detector.

    Science.gov (United States)

    Zhong, Wei-Fang; Tong, Wing-Sum; Zhou, Shan-Shan; Yip, Ka-Man; Li, Song-Lin; Zhao, Zhong-Zhen; Xu, Jun; Chen, Hu-Biao

    2017-10-01

    Bai-Hu-Tang (BHT), a classic traditional Chinese medicine (TCM) formula used for clearing heat and promoting body fluid, consists of four traditional Chinese medicines, i.e., Gypsum Fibrosum (Shigao), Anemarrhenae Rhizoma (Zhimu), Glycyrrhizae Radix et Rhizoma Praeparata cum Melle (Zhigancao), and nonglutinous rice (Jingmi). The chemical composition of BHT still remains largely elusive thus far. To qualitatively and quantitatively characterize secondary metabolites and carbohydrates in BHT, here a combination of analytical approaches using ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and ultraperformance liquid chromatography coupled with photodiode array detector was developed and validated. A total of 42 secondary metabolites in BHT were tentatively or definitely identified, of which 10 major chemicals were quantified by the extracting ion mode of quadrupole time-of-flight mass spectrometry. Meanwhile, polysaccharides, oligosaccharides, and monosaccharides in BHT were also characterized via sample pretreatment followed by sugar composition analysis. The quantitative results indicated that the determined chemicals accounted for 35.76% of the total extract of BHT, which demonstrated that the study could be instrumental in chemical dissection and quality control of BHT. The research deliverables not only laid the root for further chemical and biological evaluation of BHT, but also provided a comprehensive analytical strategy for chemical characterization of secondary metabolites and carbohydrates in traditional Chinese medicine formulas. Copyright © 2017. Published by Elsevier B.V.

  11. Qualitative and quantitative characterization of secondary metabolites and carbohydrates in Bai-Hu-Tang using ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and ultraperformance liquid chromatography coupled with photodiode array detector

    Directory of Open Access Journals (Sweden)

    Wei-Fang Zhong

    2017-10-01

    Full Text Available Bai-Hu-Tang (BHT, a classic traditional Chinese medicine (TCM formula used for clearing heat and promoting body fluid, consists of four traditional Chinese medicines, i.e., Gypsum Fibrosum (Shigao, Anemarrhenae Rhizoma (Zhimu, Glycyrrhizae Radix et Rhizoma Praeparata cum Melle (Zhigancao, and nonglutinous rice (Jingmi. The chemical composition of BHT still remains largely elusive thus far. To qualitatively and quantitatively characterize secondary metabolites and carbohydrates in BHT, here a combination of analytical approaches using ultraperformance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and ultraperformance liquid chromatography coupled with photodiode array detector was developed and validated. A total of 42 secondary metabolites in BHT were tentatively or definitely identified, of which 10 major chemicals were quantified by the extracting ion mode of quadrupole time-of-flight mass spectrometry. Meanwhile, polysaccharides, oligosaccharides, and monosaccharides in BHT were also characterized via sample pretreatment followed by sugar composition analysis. The quantitative results indicated that the determined chemicals accounted for 35.76% of the total extract of BHT, which demonstrated that the study could be instrumental in chemical dissection and quality control of BHT. The research deliverables not only laid the root for further chemical and biological evaluation of BHT, but also provided a comprehensive analytical strategy for chemical characterization of secondary metabolites and carbohydrates in traditional Chinese medicine formulas.

  12. Structural characterization of product ions of regulated veterinary drugs by electrospray ionization and quadrupole time-of-flight mass spectrometry (part 3) Anthelmintics, thyreostats, and flukicides

    Science.gov (United States)

    RATIONALE: Previously we have reported a liquid chromatography tandem mass spectrometry method for the identification and quantification of regulated veterinary drugs. The methods used three selected transition ions but most of these ions lacked structural characterization. The work presented here ...

  13. Identification of non-volatile compounds and their migration from hot melt adhesives used in food packaging materials characterized by ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Vera, Paula; Canellas, Elena; Nerín, Cristina

    2013-05-01

    The identification of unknown non-volatile migrant compounds from adhesives used in food contact materials is a very challenging task because of the number of possible compounds involved, given that adhesives are complex mixtures of chemicals. The use of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-MS/QTOF) is shown to be a successful tool for identifying non-targeted migrant compounds from two hot melt adhesives used in food packaging laminates. Out of the seven migrants identified and quantified, five were amides and one was a compound classified in Class II of the Cramer toxicity. None of the migration values exceeded the recommended Cramer exposure values.

  14. Analysis of the Constituents in “Zhu She Yong Xue Shuan Tong” by Ultra High Performance Liquid Chromatography with Quadrupole Time-of-Flight Mass Spectrometry Combined with Preparative High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Lin-Lin Wang

    2015-11-01

    Full Text Available “Zhu She Yong Xue Shuan Tong” lyophilized powder (ZSYXST, consists of a series of saponins extracted from Panax notoginseng, which has been widely used in China for the treatment of strokes. In this study, an ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS combined with preparative high performance liquid chromatography (PHPLC method was developed to rapidly identify both major and minor saponins in ZSYXST. Some high content components were removed through PHPLC in order to increase the sensitivity of the trace saponins. Then, specific characteristic fragment ions in both positive and negative mode were utilized to determine the types of aglycone, saccharide, as well as the saccharide chain linkages. As a result, 94 saponins, including 20 pairs of isomers and ten new compounds, which could represent higher than 98% components in ZSYXST, were identified or tentatively identified in commercial ZSYXST samples.

  15. Laser ablation synthesis of arsenic-phosphide Asm Pn clusters from As-P mixtures. Laser desorption ionisation with quadrupole ion trap time-of-flight mass spectrometry: The mass spectrometer as a synthesizer.

    Science.gov (United States)

    Kubáček, Pavel; Prokeš, Lubomír; Pamreddy, Annapurna; Peña-Méndez, Eladia María; Conde, José Elias; Alberti, Milan; Havel, Josef

    2018-05-30

    Only a few arsenic phosphides are known. A high potential for the generation of new compounds is offered by Laser Ablation Synthesis (LAS) and when Laser Desorption Ionization (LDI) is coupled with simultaneous Time-Of-Flight Mass Spectrometry (TOFMS), immediate identification of the clusters can be achieved. LAS was used for the generation of arsenic phosphides via laser ablation of phosphorus-arsenic mixtures while quadrupole ion trap time-of-flight mass spectrometry (QIT-TOFMS) was used to acquire the mass spectra. Many new As m P n ± clusters (479 binary and 369 mono-elemental) not yet described in the literature were generated in the gas phase and their stoichiometry determined. The likely structures for some of the observed clusters arbitrary selected (20) were computed by density functional theory (DFT) optimization. LAS is an advantageous approach for the generation of new As m P n clusters, while mass spectrometry was found to be an efficient technique for the determination of cluster stoichiometry. The results achieved might inspire the synthesis of new materials. Copyright © 2018 John Wiley & Sons, Ltd.

  16. Chiral separation and chemical profile of Dengzhan Shengmai by integrating comprehensive with multiple heart-cutting two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Sheng, Ning; Zheng, Hao; Xiao, Yao; Wang, Zhe; Li, Menglin; Zhang, Jinlan

    2017-09-29

    Chemical profile for Chinese medicine formulas composed of several herbs is always a challenge due to a big array of small molecules with high chemical diversity so much as isomers. The present paper develops a feasible strategy to characterize and identify complex chemical constituents of a four-herb traditional Chinese medicine formula, Denzhan Shenmai (DZSM) by integrating comprehensive two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC×LC-qTOF-MS) with multiple heart-cutting two-dimensional liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (MHC-qTOF-MS). DZSM was separated by C8×C18 HPLC column system for comprehensive two-dimensional liquid chromatography system and 283 compounds most of which belonged to phenolic acid, flavonoid, saponin and lignan families were characterized and identified within 75min. Some isomers and compounds at low level were analyzed on C8×Chiral HPLC column system for multiple heart-cutting two-dimensional liquid chromatography system with 1D and 2D optimized gradient elution program. These 1D cutting fractions were successively separated on 2D chiral chromatographic column under extended the 2D gradient elution time from 30s to 5.0min. 12 pairs of isomer compounds were separated with good resolution. The combination of LC×LC and MHC system provides a powerful technique for global chemical profiling of DZSM and provided feasible strategy for other complex systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Matrix-assisted laser desorption/ionization coupled with quadrupole/orthogonal acceleration time-of-flight mass spectrometry for protein discovery, identification, and structural analysis.

    Science.gov (United States)

    Baldwin, M A; Medzihradszky, K F; Lock, C M; Fisher, B; Settineri, T A; Burlingame, A L

    2001-04-15

    The design and operation of a novel UV-MALDI ionization source on a commercial QqoaTOF mass spectrometer (Applied Biosystem/MDS Sciex QSTAR Pulsar) is described. Samples are loaded on a 96-well target plate, the movement of which is under software control and can be readily automated. Unlike conventional high-energy MALDI-TOF, the ions are produced with low energies (5-10 eV) in a region of relatively low vacuum (8 mTorr). Thus, they are cooled by extensive low-energy collisions before selection in the quadrupole mass analyzer (Q1), potentially giving a quasi-continuous ion beam ideally suited to the oaTOF used for mass analysis of the fragment ions, although ion yields from individual laser shots may vary widely. Ion dissociation is induced by collisions with argon in an rf-only quadrupole cell, giving typical low-energy CID spectra for protonated peptide ions. Ions separated in the oaTOF are registered by a four-anode detector and time-to-digital converter and accumulated in "bins" that are 625 ps wide. Peak shapes depend upon the number of ion counts in adjacent bins. As expected, the accuracy of mass measurement is shown to be dependent upon the number of ions recorded for a particular peak. With internal calibration, mass accuracy better than 10 ppm is attainable for peaks that contain sufficient ions to give well-defined Gaussian profiles. By virtue of its high resolution, capability for accurate mass measurements, and sensitivity in the low-femotomole range, this instrument is ideally suited to protein identification for proteomic applications by generation of peptide tags, manual sequence interpretation, identification of modifications such as phosphorylation, and protein structural elucidation. Unlike the multiply charged ions typical of electrospray ionization, the singly charged MALDI-generated peptide ions show a linear dependence of optimal collision energy upon molecular mass, which is advantageous for automated operation. It is shown that the novel

  18. Atmospheric pressure gas chromatography coupled to quadrupole-time of flight mass spectrometry as a powerful tool for identification of non intentionally added substances in acrylic adhesives used in food packaging materials.

    Science.gov (United States)

    Canellas, E; Vera, P; Domeño, C; Alfaro, P; Nerín, C

    2012-04-27

    Acrylic adhesives are used to manufacture multilayer laminates that are used in food packaging to form the geometric shape of the package as well as to stick labels on the packages. Once applied on the packaging adhesives can supply potential migrants that could endanger the packaged food. Adhesives are complex matrices where intentionally and non intentionally added substances are present, but the identification of the migrants is required by law. In this study atmospheric pressure gas chromatography coupled to a quadrupole hyphenated to a time of flight mass spectrometer (APGC-MS/Q-TOF) has been explored for identification of unknowns coming from three different acrylic adhesives. The results are compared to those obtained by conventional GC-MS-Q (quadrupole). Sixteen compounds were identified by GC-MS/Q and five of them were confirmed by APGC-MS/Q-TOF as their molecular ions were found. Moreover, additional three new compounds were identified and their structure was elucidated working with the spectra obtained by APGC-MS/Q-TOF. This finding was very relevant as these compounds were biocides suspected to be allergenic and cytotoxic in humans. Migration studies were carried out using Tenax as solid food simulant and the results showed that the three acrylic adhesives tested in this work were safe for being used in food packaging materials since the migration of compounds previously identified was below the limit established in the current legislation. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Determination of aminoglycoside residues in milk and muscle based on a simple and fast extraction procedure followed by liquid chromatography coupled to tandem mass spectrometry and time of flight mass spectrometry.

    Science.gov (United States)

    Arsand, Juliana Bazzan; Jank, Louíse; Martins, Magda Targa; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara; Sirtori, Carla

    2016-07-01

    Antibiotics are widely used in veterinary medicine mainly for treatment and prevention of diseases. The aminoglycosides are one of the antibiotics classes that have been extensively employed in animal husbandry for the treatment of bacterial infections, but also as growth promotion. The European Union has issued strict Maximum Residue Levels (MRLs) for aminoglycosides in several animal origin products including bovine milk, bovine, swine and poultry muscle. This paper describes a fast and simple analytical method for the determination of ten aminoglycosides (spectinomycin, tobramycin, gentamicin, kanamycin, hygromycin, apramycin, streptomycin, dihydrostreptomycin, amikacin and neomycin) in bovine milk and bovine, swine and poultry muscle. For sample preparation, an extraction method was developed using trichloroacetic acid and clean up with low temperature precipitation and C18 bulk. Liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) was used to carry out quantitative analysis and liquid chromatography-quadrupole-time of flight-mass spectrometry (LC-QTOF-MS) was used to screening purposes. Both methods were validated according to the European Union Commission Directive 2002/657/EC. Good performance characteristics were obtained for recovery, precision, calibration curve, specificity, decision limits (CCα) and detection capabilities (CCβ) in all matrices evaluated. The detection limit (LOD) and quantification limit (LOQ) were ranging from 5 to 100ngg(-1) and 12.5 to 250ngg(-1), respectively. Good linearity (r)-above 0.99-was achieved in concentrations ranging from 0.0 to 2.0×MRL. Recoveries ranged from 36.8% to 98.0% and the coefficient of variation from 0.9 to 20.2%, noting that all curves have been made into their own matrices in order to minimize the matrix effects. The CCβ values obtained in qualitative method were between 25 and 250ngg(-1). The proposed method showed to be simple, easy, and adequate for high-throughput analysis of a large

  20. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo

    2016-01-01

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. - Highlights: • An UHPLC/Q-TOF tsMIM MS-based pseudotargeted metabolomics was proposed. • Compared to full scan, the improved method exhibits better repeatability and a wider linear range. • The proposed method could achieve pseudotargeted analysis on one UHPLC/Q-TOF/MS instrument. • The developed method was successfully used to discover biomarkers for alcohol-induced liver injury.

  1. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo, E-mail: jbwan@umac.mo

    2016-07-13

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. - Highlights: • An UHPLC/Q-TOF tsMIM MS-based pseudotargeted metabolomics was proposed. • Compared to full scan, the improved method exhibits better repeatability and a wider linear range. • The proposed method could achieve pseudotargeted analysis on one UHPLC/Q-TOF/MS instrument. • The developed method was successfully used to discover biomarkers for alcohol-induced liver injury.

  2. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo

    2016-07-13

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. A rapid method for simultaneous determination of 52 marker compounds in Xiao-Qing-Long-Tang by ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhou, Lei; Qi, Wen; Xu, Cong; Makino, Toshiaki; Yuan, Dan

    2014-11-01

    Xiao-Qing-Long-Tang (XQLT) is a classical Chinese medicine formula. It is generally used for the treatment of common cold, bronchial asthma, and allergic rhinitis in Asia. In this study, a multicomponent quantification fingerprinting approach based on ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry has been developed for the analysis of compounds in XQLT in 14.5 min. A total of 52 compounds were identified by co-chromatography of sample extract with authentic standards and comparing the retention time, UV spectra, molecular ions and characteristic fragment ions with those of authentic standards, or tentatively identified by MS(E) determination along with Mass Fragment software. Moreover, the method was validated for the simultaneous quantification of 16 components in XQLT commercial products. The method is practical for comprehensive standardization of XQLT and holistic comparison of its commercial products from different manufacturers. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Metabolomics Study of Resina Draconis on Myocardial Ischemia Rats Using Ultraperformance Liquid Chromatography/Quadrupole Time-of-Flight Mass Spectrometry Combined with Pattern Recognition Methods and Metabolic Pathway Analysis

    Directory of Open Access Journals (Sweden)

    Yunpeng Qi

    2013-01-01

    Full Text Available Resina draconis (bright red resin isolated from Dracaena cochinchinensis, RD has been clinically used for treatment of myocardial ischemia (MI for many years. However, the mechanisms of its pharmacological action on MI are still poorly understood. This study aimed to characterize the plasma metabolic profiles of MI and investigate the mechanisms of RD on MI using ultraperformance liquid chromatography/quadrupole time-of-flight mass spectrometry-based metabolomics combined with pattern recognition methods and metabolic pathway analysis. Twenty metabolite markers characterizing metabolic profile of MI were revealed, which were mainly involved in aminoacyl-tRNA biosynthesis, phenylalanine, tyrosine, and tryptophan biosynthesis, vascular smooth muscle contraction, sphingolipid metabolism, and so forth. After RD treatment, however, levels of seven MI metabolite markers, including phytosphingosine, sphinganine, acetylcarnitine, cGMP, cAMP, L-tyrosine, and L-valine, were turned over, indicating that RD is likely to alleviate MI through regulating the disturbed vascular smooth muscle contraction, sphingolipid metabolism, phenylalanine metabolism, and BCAA metabolism. To our best knowledge, this is the first comprehensive study to investigate the mechanisms of RD for treating MI, from a metabolomics point of view. Our findings are very valuable to gain a better understanding of MI metabolic profiles and provide novel insights for exploring the mechanisms of RD on MI.

  5. Indirect enantioseparation of fluoxetine in mouse serum by derivatization with 1R-(-)-menthyl chloroformate followed by ultra high performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhao, Jing; Jin, Yan; Shin, Yujin; Jeong, Kyung Min; Lee, Jeongmi

    2016-03-01

    Here we describe a simple and sensitive analytical method for the enantioselective quantification of fluoxetine in mouse serum using ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry. The sample preparation method included a simple deproteinization with acetonitrile in 50 μL of serum, followed by derivatization of the extracts in 50 μL of 2 mM 1R-(-)-menthyl chloroformate at 45ºC for 55 min. These conditions were statistically optimized through response surface methodology using a central composite design. Under the optimized conditions, neither racemization nor kinetic resolution occurred. The derivatized diastereomers were readily resolved on a conventional sub-2 μm C18 column under a simple gradient elution of aqueous methanol containing 0.1% formic acid. The established method was validated and found to be linear, precise, and accurate over the concentration range of 5.0-1000.0 ng/mL for both R and S enantiomers (r(2) > 0.993). Stability tests of the prepared samples at three different concentration levels showed that the R- and S-fluoxetine derivatives were relatively stable for 48 h. No significant matrix effects were observed. Last, the developed method was successfully used for enantiomeric analysis of real serum samples collected at a number of time points from mice administered with racemic fluoxetine. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. A new ultrahigh performance liquid chromatography with diode array detection coupled to electrospray ionization and quadrupole time-of-flight mass spectrometry analytical strategy for fast analysis and improved characterization of phenolic compounds in apple products.

    Science.gov (United States)

    Ramirez-Ambrosi, M; Abad-Garcia, B; Viloria-Bernal, M; Garmon-Lobato, S; Berrueta, L A; Gallo, B

    2013-11-05

    A new, rapid, selective and sensitive ultrahigh performance liquid chromatography with diode array detection coupled to electrospray ionization and quadrupole time-of-flight mass spectrometry (UHPLC-DAD-ESI-Q-ToF-MS) strategy using automatic and simultaneous acquisition of exact mass at high and low collision energy, MS(E), has been developed to obtain polyphenolic profile of apples, apple pomace and apple juice from Asturian cider apples in a single run injection of 22 min. MS(E) spectral data acquisition overcomes chromatographic co-elution problems, performing simultaneous collection of precursor ions as well as other ions produced as a result of their fragmentation, which allows resolving complex spectra from mixtures of precursor ions in an unsupervised way and eases their interpretation. Using this technique, 52 phenolic compounds of five different classes were readily characterized in these apple extracts in both positive and negative ionization modes. The spectral data for phenolic compounds obtained using this acquisition mode are comparable to those obtained by conventional LC-MS/MS as exemplified in this work. Among the 52 phenolic compounds identified in this work, 2 dihydrochalcones and 3 flavonols have been tentatively identified for the first time in apple products. Moreover, 2 flavanols, 4 dihydrochalcones, 9 hydroxycinnamic acids and 4 flavonols had not been previously reported in apple by ToF analysis to our knowledge. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Screening of 439 Pesticide Residues in Fruits and Vegetables by Gas Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and Q-TOF Spectrum Library.

    Science.gov (United States)

    Li, Jian-Xun; Li, Xiao-Ying; Chang, Qiao-Ying; Li, Yan; Jin, Ling-He; Pang, Guo-Fang; Fan, Chun-Lin

    2018-05-03

    Because of its unique characteristics of accurate mass full-spectrum acquisition, high resolution, and fast acquisition rates, GC-quadrupole-time-of-flight MS (GC-Q-TOF/MS) has become a powerful tool for pesticide residue analysis. In this study, a TOF accurate mass database and Q-TOF spectrum library of 439 pesticides were established, and the parameters of the TOF database were optimized. Through solid-phase extraction (SPE), whereby pesticides are extracted from fruit and vegetable substrates by using 40 mL 1% acetic acid in acetonitrile (v/v), purified by the Carbon/NH₂ SPE cartridge, and finally detected by GC-Q-TOF/MS, the rapid analysis of 439 pesticides in fruits and vegetables can be achieved. The methodology verification results show that more than 70 and 91% of pesticides, spiked in fruits and vegetables with concentrations of 10 and 100 μg/kg, respectively, saw recoveries that conform to the European Commission's criterion of between 70 and 120% with RSD ≤20%. Eighty-one percent of pesticides have screening detection limits lower than 10 μg/kg, which makes this a reliable analysis technology for the monitoring of pesticide residues in fruits and vegetables. This technology was further validated for its characteristics of high precision, high speed, and high throughput through successful detection of 9817 samples during 2013-2015.

  8. Liquid chromatography coupled to different atmospheric pressure ionization sources-quadrupole-time-of-flight mass spectrometry and post-column addition of metal salt solutions as a powerful tool for the metabolic profiling of Fusarium oxysporum.

    Science.gov (United States)

    Cirigliano, Adriana M; Rodriguez, M Alejandra; Gagliano, M Laura; Bertinetti, Brenda V; Godeas, Alicia M; Cabrera, Gabriela M

    2016-03-25

    Fusarium oxysporum L11 is a non-pathogenic soil-borne fungal strain that yielded an extract that showed antifungal activity against phytopathogens. In this study, reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to different atmospheric pressure ionization sources-quadrupole-time-of-flight mass spectrometry (API-QTOF-MS) was applied for the comprehensive profiling of the metabolites from the extract. The employed sources were electrospray (ESI), atmospheric pressure chemical ionization (APCI) and atmospheric pressure photoionization (APPI). Post-column addition of metal solutions of Ca, Cu and Zn(II) was also tested using ESI. A total of 137 compounds were identified or tentatively identified by matching their accurate mass signals, suggested molecular formulae and MS/MS analysis with previously reported data. Some compounds were isolated and identified by NMR. The extract was rich in cyclic peptides like cyclosporins, diketopiperazines and sansalvamides, most of which were new, and are reported here for the first time. The use of post-column addition of metals resulted in a useful strategy for the discrimination of compound classes since specific adducts were observed for the different compound families. This technique also allowed the screening for compounds with metal binding properties. Thus, the applied methodology is a useful choice for the metabolic profiling of extracts and also for the selection of metabolites with potential biological activities related to interactions with metal ions. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Identification of phase I and II metabolites of the new designer drug α-pyrrolidinohexiophenone (α-PHP) in human urine by liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS).

    Science.gov (United States)

    Paul, Michael; Bleicher, Sergej; Guber, Susanne; Ippisch, Josef; Polettini, Aldo; Schultis, Wolfgang

    2015-11-01

    Pyrrolidinophenones represent one emerging class of newly encountered drugs of abuse, also known as 'new psychoactive substances', with stimulating psychoactive effects. In this work, we report on the detection of the new designer drug α-pyrrolidinohexiophenone (α-PHP) and its phase I and II metabolites in a human urine sample of a drug abuser. Determination and structural elucidation of these metabolites have been achieved by liquid chromatography electrospray ionisation quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF-MS). By tentative identification, the exact and approximate structures of 19 phase I metabolites and nine phase II glucuronides were elucidated. Major metabolic pathways revealed the reduction of the ß-keto moieties to their corresponding alcohols, didesalkylation of the pyrrolidine ring, hydroxylation and oxidation of the aliphatic side chain leading to n-hydroxy, aldehyde and carboxylate metabolites, and oxidation of the pyrrolidine ring to its lactam followed by ring cleavage and additional hydroxylation, reduction and oxidation steps and combinations thereof. The most abundant phase II metabolites were glucuronidated ß-keto-reduced alcohols. Besides the great number of metabolites detected in this sample, α-PHP is still one of the most abundant ions together with its ß-keto-reduced alcoholic dihydro metabolite. Monitoring of these metabolites in clinical and forensic toxicology may unambiguously prove the abuse of the new designer drug α-PHP. Copyright © 2015 John Wiley & Sons, Ltd.

  10. Metabolic profiling of nuciferine in rat urine, plasma, bile and feces after oral administration using ultra-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wu, Xiao-Lei; Wu, Ming-Jiang; Chen, Xin-Ze; Ma, Hao-Ling; Ding, Li-Qin; Qiu, Feng; Pan, Qin; Zhang, De-Qin

    2017-06-05

    Nuciferine, a major alkaloid found in Nelumbinis Folium, exhibits a broad spectrum of bioactivities, such as antiobesity, anti-diabetes and anti-inflammatory. However, many research regarding nuciferine focused on the extraction, isolation and biological activity, the metabolism is not comprehensively explained in vivo. Thence, the present of this paper is to establish a simple method for speculating metabolites of nuciferine. A total of 15 metabolites were detected and tentatively identified through ultra high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry (UHPLC-DAD-QTOF-MS), including 7 new metabolites. Among them, we also discovered a previously unmentioned metabolically active site at the C 1 -OCH 3 position. These metabolites suggested that demethylation, oxidation, glucuronidation and sulfation were major metabolic pathways. This study provided significant experiment basis for its safety estimate and valuable information about the metabolism of nuciferine, which will be advantageous for new drug development. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Short-term toxicity assessments of an antibiotic metabolite in Wistar rats and its metabonomics analysis by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Han, Hongxing; Xiao, Hailong; Lu, Zhenmei

    2016-02-15

    4-Epi-oxytetracycline (4-EOTC), one of main oxytetracycline (OTC) metabolites, can be commonly detected in food and environment. The toxicity and effects of OTC on animals have been well characterized; however, its metabolites have never been studied systemically. This study aims to investigate 15-day oral dose toxicity and urine metabonomics changes of 4-EOTC after repeated administration in Wistar rats at daily doses of 0.5, 5.0 and 50.0mg/kg bw (bodyweight). Hematology and clinical chemistry parameters, including white blood cell count, red blood cell count, total protein, globulin and albumin/globulin, were obviously altered in rats of 5.0 and 50.0mg/kg bw. Histopathology changes of kidney and liver tissues were also observed in high-dose groups. Urinary metabolites from all groups were analyzed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Seventeen metabolites contributing to the clusters were identified as potential biomarkers from multivariate analysis, including aminoadipic acid, 6-phosphogluconate, sebacic acid, pipecolic acid, etc. The significant changes of these biomarkers demonstrated metabonomic variations in treated rats, especially lysine and purine metabolism. For the first time in this paper, we combined the results of toxicity and metabonomics induced by 4-EOTC for the serious reconsideration of the safety and potential risks of antibiotics and its degradation metabolites. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Identification and analysis of chemical constituents and rat serum metabolites in Suan-Zao-Ren granule using ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry combined with multiple data processing approaches.

    Science.gov (United States)

    Du, Yiyang; He, Bosai; Li, Qing; He, Jiao; Wang, Di; Bi, Kaishun

    2017-07-01

    Suan-Zao-Ren granule is widely used to treat insomnia in China. However, because of the complexity and diversity of the chemical compositions in traditional Chinese medicine formula, the comprehensive analysis of constituents in vitro and in vivo is rather difficult. In our study, an ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry and the PeakView® software, which uses multiple data processing approaches including product ion filter, neutral loss filter, and mass defect filter, method was developed to characterize the ingredients and rat serum metabolites in Suan-Zao-Ren granule. A total of 101 constituents were detected in vitro. Under the same analysis conditions, 68 constituents were characterized in rat serum, including 35 prototype components and 33 metabolites. The metabolic pathways of main components were also illustrated. Among them, the metabolic pathways of timosaponin AI were firstly revealed. The bioactive compounds mainly underwent the phase I metabolic pathways including hydroxylation, oxidation, hydrolysis, and phase II metabolic pathways including sulfate conjugation, glucuronide conjugation, cysteine conjugation, acetycysteine conjugation, and glutathione conjugation. In conclusion, our results showed that this analysis approach was extremely useful for the in-depth pharmacological research of Suan-Zao-Ren granule and provided a chemical basis for its rational. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Analysis of Therapeutic Effect of Ilex hainanensis Merr. Extract on Nonalcoholic Fatty Liver Disease through Urine Metabolite Profiling by Ultraperformance Liquid Chromatography/Quadrupole Time of Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jing-jing Li

    2013-01-01

    Full Text Available Nonalcoholic fatty liver disease (NAFLD, the most common form of chronic liver disease, is increased worldwide in parallel with the obesity epidemic. Our previous studies have showed that the extract of I. hainanensis (EIH can prevent NAFLD in rat fed with high-fat diet. In this work, we aimed to find biomarkers of NAFLD and investigate the therapeutic effects of EIH. NAFLD model was induced in male Sprague-Dawley rats by high-fat diet. The NAFLD rats were administered EIH orally (250 mg/kg for two weeks. After the experimental period, samples of 24 h urine were collected and analyzed by ultraperformance liquid chromatography/quadrupole time of flight mass spectrometry (UPLC-Q-TOF. Orthogonal partial least squares analysis (OPLSs models were built to find biomarkers of NAFLD and investigate the therapeutic effects of EIH. 22 metabolites, which are distributed in several metabolic pathways, were identified as potential biomarkers of NAFLD. Taking these biomarkers as screening indexes, EIH could reverse the pathological process of NAFLD through regulating the disturbed pathway of metabolism. The metabolomic results not only supply a systematic view of the development and progression of NAFLD but also provide a theoretical basis for the prevention or treatment of NAFLD.

  14. The Profiling and Identification of the Absorbed Constituents and Metabolites of Guizhi Decoction in Rat Plasma and Urine by Rapid Resolution Liquid Chromatography Combined with Quadrupole-Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Xiang, Hongjun; Zhang, Lishi; Song, Jiannan; Fan, Bin; Nie, Yinglan; Bai, Dong; Lei, Haimin

    2016-01-01

    Guizhi decoction (GZD), a well-known traditional Chinese medicine (TCM) prescription consisting of Ramulus Cinnamomi, Radix Paeoniae Alba, Radix Glycyrrhizae, Fructus Jujubae and Rhizoma Zingiberis Recens, is usually used for the treatment of common colds, influenza, and other pyretic conditions in the clinic. However, the absorbed ingredients and metabolic compounds of GZD have not been reported. In this paper, a method incorporating rapid resolution liquid chromatography (RRLC) with quadrupole-time-of-flight mass spectrometry (Q-TOF-MS) was used to identify ingredients after oral administration of GZD. Identification of the primary components in GZD, drug-containing serum and urine samples was carried out in order to investigate the assimilation and metabolites of the decoction in vivo. By comparing the total ion chromatograms (TICs) of GZD, a total of 71 constituents were detected or characterized. By comparing TICs of blank and dosed rat plasma, a total of 15 constituents were detected and identified as prototypes according to their retention time (tR) and MS, MS/MS data. Based on this, neutral loss scans of 80 and 176 Da in samples of rat plasma and urine helped us to identify most of the metabolites. Results showed that the predominant metabolic pathways of (epi) catechin and gallic acid were sulfation, methylation, glucuronidation and dehydroxylation; the major metabolic pathways of flavone were hydrolysis, sulfation and glucuronidation. Furthermore, degradation, oxidation and ring fission were found to often occur in the metabolism process of GZD in vivo. PMID:27626411

  15. Investigation of the Effect of Rice Wine on the Metabolites of the Main Components of Herbal Medicine in Rat Urine by Ultrahigh-Performance Liquid Chromatography-Quadrupole/Time-of-Flight Mass Spectrometry: A Case Study on Cornus officinalis

    Directory of Open Access Journals (Sweden)

    Gang Cao

    2013-01-01

    Full Text Available Ultrahigh-performance liquid chromatography-quadrupole/time-of-flight mass spectrometry (UPLC-QTOF/MS was developed for rapid and sensitive analysis of the effect of rice wine on the metabolites of the main components of herbal medicine in rat urine. Using Cornus officinalis as a model of herbal medicine, the metabolite profiles of crude and processed (steaming the crude drug presteeped in rice wine Cornus officinalis extracts in rat urine were investigated. The metabolites of Cornus officinalis were identified by using dynamic adjustment of the fragmentor voltage to produce structure-relevant fragment ions. In this work, we identified the parent compounds and metabolites of crude and processed Cornus officinalis in rats. In total, three parent compounds and seventeen new metabolites of Cornus officinalis were found in rats. The contents of the parent compounds and metabolites in vivo varied significantly after intragastric (i.g. administration of aqueous extracts of crude and processed Cornus officinalis. Data from this study suggests that UPLC-QTOF/MS could be used as a potential tool for uncovering the effects of excipients found in the metabolites of the main components of herbal medicine, in vivo, to predict and discover the processing mechanisms of herbal medicine.

  16. Comprehensive Characterization of Extractable and Nonextractable Phenolic Compounds by High-Performance Liquid Chromatography-Electrospray Ionization-Quadrupole Time-of-Flight of a Grape/Pomegranate Pomace Dietary Supplement.

    Science.gov (United States)

    Pérez-Ramírez, Iza F; Reynoso-Camacho, Rosalía; Saura-Calixto, Fulgencio; Pérez-Jiménez, Jara

    2018-01-24

    Grape and pomegranate are rich sources of phenolic compounds, and their derived products could be used as ingredients for the development of functional foods and dietary supplements. However, the profile of nonextractable or macromolecular phenolic compounds in these samples has not been evaluated. Here, we show a comprehensive characterization of extractable and nonextractable phenolic compounds of a grape/pomegranate pomace dietary supplement using high-performance liquid chromatography-electrospray ionization-quadrupole time-of-flight (HPLC-ESI-QTOF) and matrix-assisted laser desorption/ionization (MALDI)-TOF techniques. The main extractable phenolic compounds were several anthocyanins (principally malvidin 3-O-glucoside) as well as gallotannins and gallagyl derivatives; some phenolic compounds were reported in grape or pomegranate for the first time. Additionally, there was a high proportion of nonextractable phenolic compounds, including vanillic acid, and dihydroxybenzoic acid. Unidentified polymeric structures were detected by MALDI-TOF MS analysis. This study shows that mixed grape and pomegranate pomaces are a source of different classes of phenolic compounds including a high proportion of nonextractable phenolic compounds.

  17. Determination of perfluorinated alkyl acids in corn, popcorn and popcorn bags before and after cooking by focused ultrasound solid-liquid extraction, liquid chromatography and quadrupole-time of flight mass spectrometry.

    Science.gov (United States)

    Moreta, Cristina; Tena, María Teresa

    2014-08-15

    An analytical method is proposed to determine ten perfluorinated alkyl acids (PFAAs) [nine perfluorocarboxylic acids (PFCAs) and perfluorooctane sulfonate (PFOS)] in corn, popcorn and microwave popcorn packaging by focused ultrasound solid-liquid extraction (FUSLE) and ultra high performance liquid chromatography (UHPLC) coupled to quadrupole-time of flight mass spectrometry (QTOF-MS/MS). Selected PFAAs were extracted efficiently in only one 10-s cycle by FUSLE, a simple, safe and inexpensive technique. The developed method was validated for microwave popcorn bags matrix as well as corn and popcorn matrices in terms of linearity, matrix effect error, detection and quantification limits, repeatability and recovery values. The method showed good accuracy with recovery values around 100% except for the lowest chain length PFAAs, satisfactory reproducibility with RSDs under 16%, and sensitivity with limits of detection in the order of hundreds picograms per gram of sample (between 0.2 and 0.7ng/g). This method was also applied to the analysis of six microwave popcorn bags and the popcorn inside before and after cooking. PFCAs contents between 3.50ng/g and 750ng/g were found in bags, being PFHxA (perfluorohexanoic acid) the most abundant of them. However, no PFAAs were detected either corn or popcorn, therefore no migration was assumed. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Tissue-specific metabolite profiling of Cyperus rotundus L. rhizomes and (+)-nootkatone quantitation by laser microdissection, ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry, and gas chromatography-mass spectrometry techniques.

    Science.gov (United States)

    Jaiswal, Yogini; Liang, Zhitao; Guo, Ping; Ho, Hing-Man; Chen, Hubiao; Zhao, Zhongzhen

    2014-07-23

    Cyperus rotundus L. is a plant species commonly found in both India and China. The caused destruction of this plant is of critical concern for agricultural produce. Nevertheless, it can serve as a potential source of the commercially important sesquiterpenoid (+)-nootkatone. The present work describes comparative metabolite profiling and (+)-nootkatone content determination in rhizome samples collected from these two countries. Laser dissected tissues, namely, the cortex, hypodermal fiber bundles, endodermis, amphivasal vascular bundles, and whole rhizomes were analyzed by ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Gas chromatography-mass spectrometry (GC-MS) analysis was used for profiling of essential oil constituents and quantitation of (+)-nootkatone. The content of (+)-nootkatone was found to be higher in samples from India (30.47 μg/10 g) compared to samples from China (21.72 μg/10 g). The method was validated as per International Conference on Harmonisation (ICH) guidelines (Q2 R1). The results from this study can be applied for quality control and efficient utilization of this terpenoid-rich plant for several applications in food-based industries.

  19. Reaction of β-blockers and β-agonist pharmaceuticals with aqueous chlorine. Investigation of kinetics and by-products by liquid chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Quintana, José Benito; Rodil, Rosario; Cela, Rafael

    2012-06-01

    The degradation of two β-blockers (atenolol and propranolol) and one β-receptor agonist (salbutamol) during water chlorination was investigated by liquid chromatography-mass spectrometry (LC-MS). An accurate-mass quadrupole time-of-flight system (QTOF) was used to follow the time course of the pharmaceuticals and also used in the identification of the by-products. The degradation kinetics of these drugs was investigated at different concentrations of chlorine, bromide and sample pH by means of a Box-Behnken experimental design. Depending on these factors, dissipation half-lives varied in the ranges 68-145 h for atenolol, 1.3-33 min for salbutamol and 42-8362 min for propranolol. Normally, an increase in chlorine dosage and pH resulted in faster degradation of these pharmaceuticals. Moreover, the presence of bromide in water samples also resulted in a faster transformation of atenolol at low chlorine doses. The use of an accurate-mass high-resolution LC-QTOF-MS system permitted the identification of a total of 14 by-products. The transformation pathway of β-blockers/agonists consisted mainly of halogenations, hydroxylations and dealkylations. Also, many of these by-products are stable, depending on the chlorination operational parameters employed.

  20. Combined use of liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) and high performance liquid chromatography with photodiode array detector (HPLC-DAD) in systematic toxicological analysis.

    Science.gov (United States)

    Broecker, Sebastian; Pragst, Fritz; Bakdash, Abdulsallam; Herre, Sieglinde; Tsokos, Michael

    2011-10-10

    Time of flight mass spectrometry provides new possibilities of substance identification by determination of the molecular formula from accurate molecular mass and isotope pattern. However, the huge number of possible isomers requires additional evidence. As a suitable way for routine performance of systematic toxicological analysis, a method for combined use of liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) and high performance liquid chromatography with diode array detector (HPLC-DAD) was developed and applied to blood samples from 77 death cases. The blood samples were prepared by extraction with CH(2)Cl(2) and by protein precipitation with acetonitrile (1:4 (v/v)). The evaporated extracts were reconstituted in 35% acetonitril/0.1% formic acid/H(2)O and aliquots were injected for analysis by LC-QTOF-MS (Agilent 6530) and HPLC-DAD (Agilent 1200). A valve switching system enabled simultaneous operation of both separated chromatographic lines under their respective optimal conditions using the same autosampler. The ESI-QTOF-MS instrument was run in data dependent acquisition mode with switching between MS and MS/MS (cycle time 1.1s) and measuring the full mass spectra and the collision induced dissociation (CID) fragment spectra of all essential [M+H](+) ions. Libraries of accurate mass CID spectra (~2500 substances) and of DAD-UV spectra (~3300 substances) of the authors were used for substance identification. The application of this procedure is demonstrated in detail at four examples with multiple drug intake or administration. In the 77 cases altogether 198 substances were identified (87 by DAD and 195 by QTOF-MS) with a frequency between 1 and 20. In practical application, the sample preparation proved to be suitable for both techniques and for a wide variety of substances with different polarity. The automatic performance of the measurements was efficient and robust. Mutual confirmation, decrease of false positive and

  1. Method for the elucidation of the elemental composition of low molecular mass chemicals using exact masses of product ions and neutral losses: application to environmental chemicals measured by liquid chromatography with hybrid quadrupole/time-of-flight mass spectrometry.

    Science.gov (United States)

    Suzuki, Shigeru; Ishii, Tetsuko; Yasuhara, Akio; Sakai, Shinichi

    2005-01-01

    A method for elucidating the elemental compositions of low molecular weight chemicals, based primarily on mass measurements made using liquid chromatography (LC) with time-of-flight mass spectrometry (TOFMS) and quadrupole/time-of-flight mass spectrometry (LC/QTOFMS), was developed and tested for 113 chemicals of environmental interest with molecular masses up to approximately 400 Da. As the algorithm incorporating the method is not affected by differences in the instrument used, or by the ionization method and other ionization conditions, the method is useful not only for LC/TOFMS, but also for all kinds of mass spectra measured with higher accuracy and precision (uncertainties of a few mDa) employing all ionization methods and on-line separation techniques. The method involves calculating candidate compositions for intact ionized molecules (ionized forms of the sample molecule that have lost or gained no more than a proton, i.e., [M+H](+) or [M-H](-)) as well as for fragment ions and corresponding neutral losses, and eliminating those atomic compositions for the molecules that are inconsistent with the corresponding candidate compositions of fragment ions and neutral losses. Candidate compositions were calculated for the measured masses of the intact ionized molecules and of the fragment ions and corresponding neutral losses, using mass uncertainties of 2 and 5 mDa, respectively. Compositions proposed for the ionized molecule that did not correspond to the sum of the compositions of a candidate fragment ion and its corresponding neutral loss were discarded. One, 2-5, 6-10, 11-20, and >20 candidate compositions were found for 65%, 39%, 1%, 1%, and 0%, respectively, for the 124 ionized molecules formed from the 113 chemicals tested (both positive and negative ions were obtained from 11 of the chemicals). However, no candidate composition was found for 2% of the test cases (i.e., 3 chemicals), for each of which the measured mass of one of the product ions was in

  2. Screening of 485 Pesticide Residues in Fruits and Vegetables by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry Based on TOF Accurate Mass Database and QTOF Spectrum Library.

    Science.gov (United States)

    Pang, Guo-Fang; Fan, Chun-Lin; Chang, Qiao-Ying; Li, Jian-Xun; Kang, Jian; Lu, Mei-Ling

    2018-03-22

    This paper uses the LC-quadrupole-time-of-flight MS technique to evaluate the behavioral characteristics of MSof 485 pesticides under different conditions and has developed an accurate mass database and spectra library. A high-throughput screening and confirmation method has been developed for the 485 pesticides in fruits and vegetables. Through the optimization of parameters such as accurate mass number, time of retention window, ionization forms, etc., the method has improved the accuracy of pesticide screening, thus avoiding the occurrence of false-positive and false-negative results. The method features a full scan of fragments, with 80% of pesticide qualitative points over 10, which helps increase pesticide qualitative accuracy. The abundant differences of fragment categories help realize the effective separation and qualitative identification of isomer pesticides. Four different fruits and vegetables-apples, grapes, celery, and tomatoes-were chosen to evaluate the efficiency of the method at three fortification levels of 5, 10, and 20 μg/kg, and satisfactory results were obtained. With this method, a national survey of pesticide residues was conducted between 2012 and 2015 for 12 551 samples of 146 different fruits and vegetables collected from 638 sampling points in 284 counties across 31 provincial capitals/cities directly under the central government, which provided scientific data backup for ensuring pesticide residue safety of the fruits and vegetables consumed daily by the public. Meanwhile, the big data statistical analysis of the new technique also further proves it to be of high speed, high throughput, high accuracy, high reliability, and high informatization.

  3. Short-term toxicity assessments of an antibiotic metabolite in Wistar rats and its metabonomics analysis by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Han, Hongxing; Xiao, Hailong; Lu, Zhenmei

    2016-01-01

    4-Epi-oxytetracycline (4-EOTC), one of main oxytetracycline (OTC) metabolites, can be commonly detected in food and environment. The toxicity and effects of OTC on animals have been well characterized; however, its metabolites have never been studied systemically. This study aims to investigate 15-day oral dose toxicity and urine metabonomics changes of 4-EOTC after repeated administration in Wistar rats at daily doses of 0.5, 5.0 and 50.0 mg/kg bw (bodyweight). Hematology and clinical chemistry parameters, including white blood cell count, red blood cell count, total protein, globulin and albumin/globulin, were obviously altered in rats of 5.0 and 50.0 mg/kg bw. Histopathology changes of kidney and liver tissues were also observed in high-dose groups. Urinary metabolites from all groups were analyzed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Seventeen metabolites contributing to the clusters were identified as potential biomarkers from multivariate analysis, including aminoadipic acid, 6-phosphogluconate, sebacic acid, pipecolic acid, etc. The significant changes of these biomarkers demonstrated metabonomic variations in treated rats, especially lysine and purine metabolism. For the first time in this paper, we combined the results of toxicity and metabonomics induced by 4-EOTC for the serious reconsideration of the safety and potential risks of antibiotics and its degradation metabolites. - Highlights: • 4-Epioxytetracycline (4-EOTC) induced damages in liver and kidney. • Metabonomics changes especially amino acid and purine metabolism were observed. • Security of OTC metabolite 4-EOTC should be taken into serious reconsideration.

  4. Metabonomics study of the therapeutic mechanism of fenugreek galactomannan on diabetic hyperglycemia in rats, by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Jiang, Wenyue; Gao, Lu; Li, Pengdong; Kan, Hong; Qu, Jiale; Men, Lihui; Liu, Zhiqiang; Liu, Zhongying

    2017-02-15

    Fenugreek is a traditional plant for the treatment of diabetes. Galactomannan, an active major component in fenugreek seeds, has shown hypoglycemic activity. The present study was performed to investigate the therapeutic mechanism underlying fenugreek galactomannan (F-GAL) in treating diabetes, using a metabonomics approach based on ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS). The F-GAL used for study was highly purified, and its yield, purity, and galactose/mannose ratio were characterized by capillary zone electrophoresis (CZE) and a modified phenol-sulfuric acid method. After treatment of streptozotocin (STZ)-induced diabetic rats with F-GAL for 28days, urine and serum samples were analyzed by UPLC-QTOF/MS. Multivariate statistical approaches such as principal component analysis (PCA) and orthogonal projection to latent structures squares-discriminant analysis (OPLS-DA) were applied to distinguish the non-diabetic/untreated, diabetic/untreated, and diabetic/F-GAL-treated groups. Then, potential biomarkers were identified that may help elucidate the underlying therapeutic mechanism of F-GAL in diabetes. The results demonstrated that there was a clear separation among the three groups in the PCA model. Fourteen potential biomarkers were identified by OPLS-DA, and they were determined to be produced in response to the therapeutic effects of F-GAL. These biomarkers were involved in histidine metabolism, tryptophan metabolism, energy metabolism, phenylalanine metabolism, sphingolipid metabolism, glycerophospholipid metabolism, and arachidonic acid metabolism. In conclusion, our study demonstrates that a metabonomics approach is a powerful, novel tool that can be used to evaluate the underlying therapeutic mechanisms of herb extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Screening for in vitro metabolites of kakkalide and irisolidone in human and rat intestinal bacteria by ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Guozhe; Gong, Tianxing; Kano, Yoshihiro; Yuan, Dan

    2014-02-01

    Kakkalide and irisolidone, the main isoflavones of Flos Puerariae, exhibit a wide spectrum of bioactivities. Intestinal bacteria biotransformation plays an important role in the metabolic pathways of flavones, and is directly related to the bioactivities of the prodrugs after oral administration. To the best of our knowledge, the metabolic pathways of kakkalide and irisolidone in vitro have not been comprehensively studied yet. This paper describes the strategy using ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF MS) for the rapid analysis of the metabolic profiles of kakkalide and irisolidone after incubated with human and rat intestinal bacteria. Bacteria incubated samples were prepared and analyzed after incubated under anaerobic conditions for 48 h. A total of 17 metabolites, including parent compounds, were detected in human and rat intestinal bacteria incubated samples. The results obtained indicate that hydrolysis, dehydroxylation, demethoxylation, demethylation, hydroxylation, decarbonylation, and reduction were the detected metabolic pathways of kakkalide and irisolidone in vitro. The conversion rate of irisolidone in human and rat bacteria was 8.57% and 6.51%, respectively. Biochanin A was the relatively main metabolite of irisolidone, and the content of biochanin A in human and rat bacteria was 3.68% and 4.25%, respectively. The conversion rate of kakkalide in human and rat bacteria was 99.92% and 98.58%, respectively. Irisolidone was the main metabolite of kakkalide, and the content of irisolidone in human and rat bacteria was 89.58% and 89.38%, respectively. This work not only provides the evidence of kakkalide and irisolidone metabolites in vivo, but also demonstrates a simple, fast, sensitive, and inexpensive method for identification of metabolites of other compounds transformed by intestinal bacteria. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Rapid wide-scope screening of drugs of abuse, prescription drugs with potential for abuse and their metabolites in influent and effluent urban wastewater by ultrahigh pressure liquid chromatography-quadrupole-time-of-flight-mass spectrometry

    International Nuclear Information System (INIS)

    Hernandez, Felix; Bijlsma, Lubertus; Sancho, Juan V.; Diaz, Ramon; Ibanez, Maria

    2011-01-01

    This work illustrates the potential of hybrid quadrupole-time-of-flight mass spectrometry (QTOF MS) coupled to ultrahigh pressure liquid chromatography (UHPLC) to investigate the presence of drugs of abuse in wastewater. After solid-phase extraction with Oasis MCX cartridges, seventy-six illicit drugs, prescription drugs with potential for abuse, and metabolites were investigated in the samples by TOF MS using electrospray interface under positive ionization mode, with MS data acquired over an m/z range of 50-1000 Da. For 11 compounds, reference standards were available, and experimental data (e.g., retention time and fragmentation data) could be obtained, facilitating a more confident identification. The use of a QTOF instrument enabled the simultaneous application of two acquisition functions with different collision energies: a low energy (LE) function, where none or poor fragmentation took place, and a high energy (HE) function, where fragmentation in the collision cell was promoted. This approach, known as MS E , enabled the simultaneous acquisition of full-spectrum accurate mass data of both protonated molecules and fragment ions in a single injection, providing relevant information that facilitates the rapid detection and reliable identification of these emerging contaminants in the sample matrices analyzed. In addition, isomeric compounds, like the opiates, morphine and norcodeine, could be discriminated by their specific fragments observed in HE TOF MS spectra, without the need of reference standards. UHPLC-QTOF MS was proven to be a powerful and efficient technique for rapid wide-scope screening and identification of many relevant drugs in complex matrices, such as influent and effluent urban wastewater.

  7. Rapid wide-scope screening of drugs of abuse, prescription drugs with potential for abuse and their metabolites in influent and effluent urban wastewater by ultrahigh pressure liquid chromatography-quadrupole-time-of-flight-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez, Felix, E-mail: felix.hernandez@qfa.uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellon (Spain); Bijlsma, Lubertus, E-mail: bijlsma@guest.uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellon (Spain); Sancho, Juan V.; Diaz, Ramon; Ibanez, Maria [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellon (Spain)

    2011-01-17

    This work illustrates the potential of hybrid quadrupole-time-of-flight mass spectrometry (QTOF MS) coupled to ultrahigh pressure liquid chromatography (UHPLC) to investigate the presence of drugs of abuse in wastewater. After solid-phase extraction with Oasis MCX cartridges, seventy-six illicit drugs, prescription drugs with potential for abuse, and metabolites were investigated in the samples by TOF MS using electrospray interface under positive ionization mode, with MS data acquired over an m/z range of 50-1000 Da. For 11 compounds, reference standards were available, and experimental data (e.g., retention time and fragmentation data) could be obtained, facilitating a more confident identification. The use of a QTOF instrument enabled the simultaneous application of two acquisition functions with different collision energies: a low energy (LE) function, where none or poor fragmentation took place, and a high energy (HE) function, where fragmentation in the collision cell was promoted. This approach, known as MS{sup E}, enabled the simultaneous acquisition of full-spectrum accurate mass data of both protonated molecules and fragment ions in a single injection, providing relevant information that facilitates the rapid detection and reliable identification of these emerging contaminants in the sample matrices analyzed. In addition, isomeric compounds, like the opiates, morphine and norcodeine, could be discriminated by their specific fragments observed in HE TOF MS spectra, without the need of reference standards. UHPLC-QTOF MS was proven to be a powerful and efficient technique for rapid wide-scope screening and identification of many relevant drugs in complex matrices, such as influent and effluent urban wastewater.

  8. Ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry based chemical profiling approach for the holistic quality control of complex Kang-Jing formula preparations.

    Science.gov (United States)

    Yang, Xiao-Huan; Cheng, Xiao-Lan; Qin, Bing; Cai, Zhuo-Ya; Cai, Xiong; Liu, Shao; Wang, Qi; Qin, Yong

    2016-05-30

    The Kang-Jing (KJ) formula is a compound preparation made from 12 kinds of herbs. So far, four different methods (M1-M4) have been documented for KJ preparation, but the influence of preparation methods on the holistic quality of KJ have remained unknown. In this study, a strategy was proposed to investigate the influence of different preparation methods on the holistic quality of KJ using ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry (UHPLC-QTOF-MS/MS) based chemical profiling. A total of 101 compounds mainly belonging to flavonoids, tanshinones, monoterpene glycosides, triterpenoid saponins, alkaloids, phenolic acids and volatile oils, were identified. Among these compounds, glaucine was detected only in M3/M4 samples, while two dehydrocorydaline isomers merely detected in M2/M3/M4 samples. Tetrahydrocolumbamine, ethylic lithospermic acid, salvianolic acid E and rosmarimic acid were only detected in M1/M3/M4 samples. In the subsequent quantitative analysis, 12 major compounds were determined by UHPLC-MS/MS. The proposed method was validated with respect to linearity, accuracy, precision and recovery. It was found that the contents of marker compounds varied significantly in samples prepared by different methods. These results demonstrated that preparation method does significantly affect the holistic quality of KJ. UHPLC-QTOF-MS/MS based chemical profiling approach is efficient and reliable for comprehensive quality evaluation of KJ. Collectively, this study provide the chemical evidence for revealing the material basis of KJ, and establish a simple and accurate chemical profiling method for its quality control. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Negative chemical ionization gas chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry and automated accurate mass data processing for determination of pesticides in fruit and vegetables.

    Science.gov (United States)

    Besil, Natalia; Uclés, Samanta; Mezcúa, Milagros; Heinzen, Horacio; Fernández-Alba, Amadeo R

    2015-08-01

    Gas chromatography coupled to high resolution hybrid quadrupole time-of-flight mass spectrometry (GC-QTOF MS), operating in negative chemical ionization (NCI) mode and combining full scan with MSMS experiments using accurate mass analysis, has been explored for the automated determination of pesticide residues in fruit and vegetables. Seventy compounds were included in this approach where 50 % of them are not approved by the EU legislation. A global 76 % of the analytes could be identified at 1 μg kg(-1). Recovery studies were developed at three concentration levels (1, 5, and 10 μg kg(-1)). Seventy-seven percent of the detected pesticides at the lowest level yielded recoveries within the 70 %-120 % range, whereas 94 % could be quantified at 5 μg kg(-1), and the 100 % were determined at 10 μg kg(-1). Good repeatability, expressed as relative standard deviation (RSD home-made database was developed and applied to an automatic accurate mass data processing. Measured mass accuracies of the generated ions were mainly less than 5 ppm for at least one diagnostic ion. When only one ion was obtained in the single-stage NCI-MS, a representative product ion from MSMS experiments was used as identification criterion. A total of 30 real samples were analyzed and 67 % of the samples were positive for 12 different pesticides in the range 1.0-1321.3 μg kg(-1).

  10. Separation and characterization of chemical constituents in Ginkgo biloba extract by off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography coupled with quadrupole-time of flight mass spectrometry.

    Science.gov (United States)

    Ji, Shuai; He, Dan-Dan; Wang, Tian-Yun; Han, Jie; Li, Zheng; Du, Yan; Zou, Jia-Hui; Guo, Meng-Zhe; Tang, Dao-Quan

    2017-11-30

    Ginkgo biloba extract (GBE), derived from the leaves of Ginkgo biloba L., is one of the most widely used traditional Chinese medicines worldwide. Due to high structural diversity and low abundance of chemical constituents in GBE, conventional reversed-phase liquid chromatography has limited power to meet the needs of its quality control. In this study, an off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography (HILIC×RP 2D-LC) system coupled with diode array detection (DAD) and quadrupole time-of-flight mass spectrometry (qTOF-MS) was established to comprehensively analyze the chemical constituents of GBE. After optimizing the chromatographic columns and mobile phase of 2D-LC, a Waters XBridge Amide column using acetonitrile/water/formic acid as the mobile phase was selected as the first dimension to fractionate GBE, and the obtained fractions were further separated on an Agilent Zorbax XDB-C18 column with methanol/water/formic acid as the mobile phase. As a result, a total of 125 compounds were detected in GBE. The orthogonality of the 2D-LC system was 69.5%, and the practical peak capacity was 3864 and 2994, respectively, calculated by two different methods. The structures of 104 compounds were tentatively characterized by qTOF-MS analysis, and 21 of them were further confirmed by comparing with reference standards. This established HILIC×RP 2D-LC-qTOF/MS system can greatly improve the separation and characterization of natural products in GBE or other complicated herbal extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Reversed-phase ultra-high-performance liquid chromatography coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometry as a powerful tool for metabolic profiling of vegetables: Lactuca sativa as an example of its application.

    Science.gov (United States)

    Abu-Reidah, I M; Contreras, M M; Arráez-Román, D; Segura-Carretero, A; Fernández-Gutiérrez, A

    2013-10-25

    Lettuce (Lactuca sativa), a leafy vegetal widely consumed worldwide, fresh cut or minimally processed, constitutes a major dietary source of natural antioxidants and bioactive compounds. In this study, reversed-phase ultra-high-performance liquid chromatography (RP-UHPLC) coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometry (ESI-QTOF-MS) was applied for the comprehensive profiling of polar and semi-polar metabolites from three lettuce cultivars (baby, romaine, and iceberg). The UHPLC systems allowed the use of a small-particle-size C18 column (1.8 μm), with very fine resolution for the separation of up to seven isomers, and the QTOF mass analyzer enabled sensitive detection with high mass resolution and accuracy in full scan. Thus, a total of 171 compounds were tentatively identified by matching their accurate mass signals and suggested molecular formula with those previously reported in family Asteraceae. Afterwards, their structures were also corroborated by the MS/MS data provided by the QTOF analyzer. Well-known amino acids, organic acids, sesquiterpene lactones, phenolic acids and flavonoids were characterized, e.g. lactucin, lactucopicrin, caftaric acid, chlorogenic acid, caffeoylmalic acid, chicoric acid, isochlorogenic acid A, luteolin, and quercetin glycosides. For this plant species, this is the first available report of several isomeric forms of the latter polyphenols and other types of components such as nucleosides, peptides, and tryptophan-derived alkaloids. Remarkably, 10 novel structures formed by the conjugation of known amino acids and sesquiterpene lactones were also proposed. Thus, the methodology applied is a useful option to develop an exhaustive metabolic profiling of plants that helps to explain their potential biological activities and folk uses. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Simultaneous detection and identification of precursors, degradation and co-products of chemical warfare agents in drinking water by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Tak, Vijay; Purohit, Ajay; Pardasani, Deepak; Goud, D Raghavender; Jain, Rajeev; Dubey, D K

    2014-11-28

    Environmental markers of chemical warfare agents (CWAs) comprise millions of chemical structures. The simultaneous detection and identification of these environmental markers poses difficulty due to their diverse chemical properties. In this work, by using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF), a generic analytical method for the detection and identification of wide range of environmental markers of CWAs (including precursors, degradation and co-products of nerve agents and sesqui-mustards) in drinking water, was developed. The chromatographic analysis of 55 environmental markers of CWAs including isomeric and isobaric compounds was accomplished within 20 min, using 1.8 μm particle size column. Subsequent identification of the compounds was achieved by the accurate mass measurement of either protonated molecule [M+H](+) or ammonium adduct [M+NH4](+) and fragment ions. Isomeric and isobaric compounds were distinguished by chromatographic retention time, characteristic fragment ions generated by both in-source collision induced dissociation (CID) and CID in the collision cell by MS/MS experiments. The exact mass measurement errors for all ions were observed less than 3 ppm with internal calibration. The method limits of detection (LODs) and limits of quantification (LOQs) were determined in drinking water and found to be 1-50 ng mL(-1) and 5-125 ng mL(-1), respectively. Applicability of the proposed method was proved by determining the environmental markers of CWAs in aqueous samples provided by Organization for the Prohibition of Chemical Weapons during 34th official proficiency test. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Short-term toxicity assessments of an antibiotic metabolite in Wistar rats and its metabonomics analysis by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Han, Hongxing [College of Life Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058 (China); Xiao, Hailong [Hangzhou Institute for Food and Drug Control, Hangzhou 310004 (China); Lu, Zhenmei, E-mail: lzhenmei@zju.edu.cn [College of Life Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058 (China)

    2016-02-15

    4-Epi-oxytetracycline (4-EOTC), one of main oxytetracycline (OTC) metabolites, can be commonly detected in food and environment. The toxicity and effects of OTC on animals have been well characterized; however, its metabolites have never been studied systemically. This study aims to investigate 15-day oral dose toxicity and urine metabonomics changes of 4-EOTC after repeated administration in Wistar rats at daily doses of 0.5, 5.0 and 50.0 mg/kg bw (bodyweight). Hematology and clinical chemistry parameters, including white blood cell count, red blood cell count, total protein, globulin and albumin/globulin, were obviously altered in rats of 5.0 and 50.0 mg/kg bw. Histopathology changes of kidney and liver tissues were also observed in high-dose groups. Urinary metabolites from all groups were analyzed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Seventeen metabolites contributing to the clusters were identified as potential biomarkers from multivariate analysis, including aminoadipic acid, 6-phosphogluconate, sebacic acid, pipecolic acid, etc. The significant changes of these biomarkers demonstrated metabonomic variations in treated rats, especially lysine and purine metabolism. For the first time in this paper, we combined the results of toxicity and metabonomics induced by 4-EOTC for the serious reconsideration of the safety and potential risks of antibiotics and its degradation metabolites. - Highlights: • 4-Epioxytetracycline (4-EOTC) induced damages in liver and kidney. • Metabonomics changes especially amino acid and purine metabolism were observed. • Security of OTC metabolite 4-EOTC should be taken into serious reconsideration.

  14. New drostanolone metabolites in human urine by liquid chromatography time-of-flight tandem mass spectrometry and their application for doping control.

    Science.gov (United States)

    Liu, Yang; Lu, Jianghai; Yang, Sheng; Zhang, Qingying; Xu, Youxuan

    2016-04-01

    Drostanolone is one of the most frequently detected anabolic androgenic steroids in doping control analysis. Here, we studied drostanolone urinary metabolic profiles using liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. The drug was administered to one healthy male volunteer and liquid-liquid extraction along with direct-injection were used to analyze urine samples. Chromatographic peaks for potential metabolites were identified with the theoretical [M-H](-) as a target ion in a full scan experiment and actual deprotonated ions were analyzed in targeted MS/MS mode. Eleven metabolites including five new sulfates, five glucuronide conjugates, and one free metabolite were confirmed for drostanolone. Due to the absence of useful fragment ions to illustrate the steroid ring structure of drostanolone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was used to obtain structural details of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and a potential structure was proposed using a combined MS approach. Metabolite detection times were recorded and S4 (2α-methyl-5α-androstan-17-one-6β-ol-3α-sulfate) and G1 (2α-methyl-5α-androstan-17-one-3α-glucuronide) were thought to be new potential biomarkers for drostanolone misuse which can be detected up to 24days by liquid-liquid extraction and 7days by direct-injection analysis after intramuscular injection. S4 and G1 were also detected in two drostanolone-positive routine urine samples. Copyright © 2016 Elsevier Inc. All rights reserved.

  15. Structural elucidation of AgAsS2 glass by the analysis of clusters formed during laser desorption ionisation applying quadrupole ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Mawale, Ravi Madhukar; Alberti, Milan; Zhang, Bo; Fraenkl, Max; Wagner, Tomas; Havel, Josef

    2016-03-15

    The structure of AgA(s)S2 glass, which has a broad range of applications, is still not well understood and a systematic mass spectrometric analysis of AgA(s)S2 glass is currently not available. Elucidation of the structure should help in the development of this material. The AgA(s)S2 glass was prepared by the melt-quenched technique. Laser desorption ionisation (LDI) using quadrupole ion trap time-of-flight mass spectrometry (QIT-TOFMS) was used to follow the generation of Ag(m)As(n)S(x) clusters. The stoichiometry of the clusters generated was determined via collision-induced dissociation (CID) and modelling of isotopic patterns. The AgA(s)S2 glass was characterised by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. The LDI of AgA(s)S2 glass leads to the formation of unary (Ag+/− and As(3+)) species, 38 binary (As(n)S(x), Ag(m)S(x)), and 98 ternary (Ag(m)As(n)S(x)) singly charged clusters. The formation of silver-rich nano-grains during AgA(s)S2 glass synthesis has been identified using TEM analysis and also verified by QIT-TOFMS. TOFMS was shown to be a useful technique to study the generation of Ag(m)As(n)S(x )clusters. SEM, TEM and EDX analysis proved that the structure of AgA(s)S2 glass is ‘grain-like’ where grains are either: (1) Silver-rich ‘islands’ (Ag(m,) m up to 39) connected by arsenic and/or sulfur or arsenic sulfide chains or (2) silver sulfide (Ag2S)m (m = 9-20) clusters also similarly inter-connected. This obtained structural information may be useful for the development of ultra-high-density phase-change storage and memory devices using this kind of glass as a base.

  16. Determination of spatial distribution of melamine-cyanuric acid crystals in rat kidney tissue by histology and imaging matrix-assisted laser desorption/ionization quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Kim, Chae-Wook; Yun, Jun-Won; Bae, Il-Hong; Lee, Joon-Seok; Kang, Hyun-Jin; Joo, Kyung-Mi; Jeong, Hye-Jin; Chung, Jin-Ho; Park, Young-Ho; Lim, Kyung-Min

    2010-01-01

    After the outbreak of acute renal failure associated with melamine-contaminated pet food, many attempts have been made to uncover the mechanism underlying the renal toxicity caused by melamine and melamine-related compounds. Using rat models, we investigated the renal crystal formation following the ingestion of a melamine-cyanuric acid mixture (M+CA, 1:1) to gain insight into the M+CA-induced renal toxicity. M+CA did not induce toxicity in precision-cut kidney slices, suggesting that M+CA does not have a direct nephrotoxicity. On the contrary, oral administration of M+CA for 3 days induced nephrotoxicity as determined by increased serum blood urea nitrogen and creatinine, reduced creatinine clearance, and enlarged kidneys in the animals treated with 50 mg/kg M+CA (melamine, 25 mg/kg, and cyanuric acid, 25 mg/kg; 2 of 10 animals) and 100 mg/kg M+CA (9 of 9 animals). While urine crystals were found in all animals treated with M+CA (25-100 mg/kg), histological examination revealed that renal crystals could be observed only in the kidneys of animals showing signs of nephrotoxicity. Remarkably, at 50 mg/kg M+CA, crystals were observed mainly in the medulla region of the kidney, while at 100 mg/kg, crystals were disseminated throughout the cortex and medulla regions. To further investigate the crystal formation by M+CA, matrix-assisted laser desorption/ionization quadrupole time-of-flight (MALDI-Q-TOF) imaging mass spectrometry detecting melamine distribution through monitoring the product ion (m/z 85, M + H) from melamine (m/z 127, M + H) was developed to directly obtain the image of melamine distribution in the kidney. The distribution image of melamine in kidney tissue confirmed that dense points of melamine were located only in the medulla region at 50 mg/kg M+CA, while at 100 mg/kg, they were disseminated widely from the cortex to medulla. These results demonstrated that M+CA ingestion could lead to crystal formation in kidney tubules along the osmotic gradient and

  17. Screening for anabolic steroids and related compounds in illegal cocktails by liquid chromatography/time-of-flight mass spectrometry and liquid chromatography/quadrupole time-of-flight tandem mass spectrometry with accurate mass measurement

    NARCIS (Netherlands)

    Nielen, M.W.F.; Vissers, J.P.C.; Fuchs, R.E.M.; Velde, van J.W.; Lommen, A.

    2001-01-01

    Findings of illegal hormone preparations such as syringes, bottles, cocktails, and so on, are an important information source for the nature of the current abuse of anabolic steroids and related compounds as growth-promoting agents in cattle. A new screening method for steroids in cocktails is

  18. New Metabolites of Coumarin Detected in Human Urine Using Ultra Performance Liquid Chromatography/Quadrupole-Time-of-Flight Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Letícia Paula Leonart

    2017-11-01

    Full Text Available Coumarin (1,2-benzopyrone is a natural compound whose metabolism in humans was established in the 1970s. However, a new metabolite was recently identified in human plasma, indicating that the metabolism of coumarin has not been completely elucidated. To complement the knowledge of its metabolism, a rapid and sensitive method using UPLC-QTOF-MS was developed. A total of 12 metabolites was identified using MetaboLynxTM software, including eight metabolites not previously reported in human urine. The identified biotransformation included hydroxylation, glucuronidation, sulfation, methylation, and conjugation with N-acetylcysteine. The present work demonstrates that the metabolism study of coumarin was incomplete, possibly due to limitations of old techniques. The identification of eight inedited metabolites of such a simple molecule suggests that the information regarding the metabolism of other drugs may also be incomplete, and therefore, new investigations are necessary.

  19. Application of targeted quantitative proteomics analysis in human cerebrospinal fluid using a liquid chromatography matrix-assisted laser desorption/ionization time-of-flight tandem mass spectrometer (LC MALDI TOF/TOF) platform.

    Science.gov (United States)

    Pan, Sheng; Rush, John; Peskind, Elaine R; Galasko, Douglas; Chung, Kathryn; Quinn, Joseph; Jankovic, Joseph; Leverenz, James B; Zabetian, Cyrus; Pan, Catherine; Wang, Yan; Oh, Jung Hun; Gao, Jean; Zhang, Jianpeng; Montine, Thomas; Zhang, Jing

    2008-02-01

    Targeted quantitative proteomics by mass spectrometry aims to selectively detect one or a panel of peptides/proteins in a complex sample and is particularly appealing for novel biomarker verification/validation because it does not require specific antibodies. Here, we demonstrated the application of targeted quantitative proteomics in searching, identifying, and quantifying selected peptides in human cerebrospinal spinal fluid (CSF) using a matrix-assisted laser desorption/ionization time-of-flight tandem mass spectrometer (MALDI TOF/TOF)-based platform. The approach involved two major components: the use of isotopic-labeled synthetic peptides as references for targeted identification and quantification and a highly selective mass spectrometric analysis based on the unique characteristics of the MALDI instrument. The platform provides high confidence for targeted peptide detection in a complex system and can potentially be developed into a high-throughput system. Using the liquid chromatography (LC) MALDI TOF/TOF platform and the complementary identification strategy, we were able to selectively identify and quantify a panel of targeted peptides in the whole proteome of CSF without prior depletion of abundant proteins. The effectiveness and robustness of the approach associated with different sample complexity, sample preparation strategies, as well as mass spectrometric quantification were evaluated. Other issues related to chromatography separation and the feasibility for high-throughput analysis were also discussed. Finally, we applied targeted quantitative proteomics to analyze a subset of previously identified candidate markers in CSF samples of patients with Parkinson's disease (PD) at different stages and Alzheimer's disease (AD) along with normal controls.

  20. ALICE Time Of Flight Detector

    CERN Multimedia

    Alici, A

    2013-01-01

    Charged particles in the intermediate momentum range are identified in ALICE by the Time Of Flight (TOF) detector. The time measurement with the TOF, in conjunction with the momentum and track length measured by the tracking detector, is used to calculate the particle mass.

  1. Development of a Tandem-Electrostatic-Quadrupole facility for Accelerator-Based Boron Neutron Capture Therapy

    International Nuclear Information System (INIS)

    Kreiner, A.J.; Castell, W.; Di Paolo, H.; Baldo, M.; Bergueiro, J.

    2011-01-01

    We describe the present status of an ongoing project to develop a Tandem-ElectroStatic-Quadrupole (TESQ) accelerator facility for Accelerator-Based (AB)-BNCT. The project final goal is a machine capable of delivering 30 mA of 2.4 MeV protons to be used in conjunction with a neutron production target based on the 7 Li(p,n) 7 Be reaction. The machine currently being constructed is a folded TESQ with a high-voltage terminal at 0.6 MV. We report here on the progress achieved in a number of different areas.

  2. Development of a Tandem-Electrostatic-Quadrupole facility for Accelerator-Based Boron Neutron Capture Therapy.

    Science.gov (United States)

    Kreiner, A J; Castell, W; Di Paolo, H; Baldo, M; Bergueiro, J; Burlon, A A; Cartelli, D; Vento, V Thatar; Kesque, J M; Erhardt, J; Ilardo, J C; Valda, A A; Debray, M E; Somacal, H R; Sandin, J C Suarez; Igarzabal, M; Huck, H; Estrada, L; Repetto, M; Obligado, M; Padulo, J; Minsky, D M; Herrera, M; Gonzalez, S J; Capoulat, M E

    2011-12-01

    We describe the present status of an ongoing project to develop a Tandem-ElectroStatic-Quadrupole (TESQ) accelerator facility for Accelerator-Based (AB)-BNCT. The project final goal is a machine capable of delivering 30 mA of 2.4 MeV protons to be used in conjunction with a neutron production target based on the (7)Li(p,n)(7)Be reaction. The machine currently being constructed is a folded TESQ with a high-voltage terminal at 0.6 MV. We report here on the progress achieved in a number of different areas. Copyright © 2011 Elsevier Ltd. All rights reserved.

  3. ALICE Time of Flight Module

    CERN Multimedia

    The Time-Of-Flight system of ALICE consists of 90 such modules, each containing 15 or 19 Multigap Resistive Plate Chamber (MRPC) strips. This detector is used for identification of charged particles. It measures with high precision (50 ps) the time of flight of charged particles and therefore their velocity. The curvature of the particle trajectory inside the magnetic field gives the momentum, thus the particle mass is calculated and the particle is identified The MRPC is a stack of resistive glass plates, separated from each other by nylon fishing line. The mass production of the chambers (~1600, covering a surface of 150 m2) was done at INFN Bologna, while the first prototypes were bult at CERN.

  4. Structural characterization of product ions by electrospray ionization and quadrupole time-of-flight mass spectrometry to support regulatory analysis of veterinary drug residues in foods Part 2: Benzimidazoles nitromidaz.....

    Science.gov (United States)

    RATIONALE: Analysis for identification and quantification of regulated veterinary drug residues in foods are usually achieved by liquid chromatography coupled to tandem mass spectrometry. The instrument method requires the selection of characteristic ions, but structure elucidation is seldom perform...

  5. Analysis of ibuprofen and its main metabolites in roots, shoots, and seeds of cowpea (Vigna unguiculata L. Walp) using liquid chromatography-quadrupole time-of-flight mass spectrometry: uptake, metabolism, and translocation.

    Science.gov (United States)

    Picó, Yolanda; Alvarez-Ruiz, Rodrigo; Wijaya, Leonard; Alfarhan, Ahmed; Alyemeni, Mohammed; Barceló, Damià

    2018-01-01

    A liquid chromatography quadruple time-of-flight mass spectrometry (LC-QqTOF-MS/MS) method was developed for simultaneous quantitative analysis of ibuprofen (IBU), 1- and 2-hydroxyibuprofen (1-OH IBU and 2-OH IBU), and carboxyibuprofen (CBX IBU) while preserving the ability of the instrument to get precursor and product ion mass spectra of non-target compounds. The trigger was the precursor ions reaching 100 cps intensity. Sample preparation was carried out by ultrasound solid-liquid extraction with methanol as extraction solvent at pH  70% for all target analytes at low and high concentration levels. The lowest limit of quantification was cowpea (Vigna unguiculata (L.) Walp) treated at high IBU concentrations and its presence in vegetables irrigated with treated water. Up to 46 metabolites, mostly hydroxylated metabolites and conjugates with hexosides and amino acids, were identified. The most abundant metabolites were also identified in an eggplant sample. Graphical Abstract ᅟ Ibuprofen metabolite identification.

  6. Improved ultra-performance liquid chromatography with electrospray ionization quadrupole-time-of-flight high-definition mass spectrometry method for the rapid analysis of the chemical constituents of a typical medical formula: Liuwei Dihuang Wan.

    Science.gov (United States)

    Wang, Ping; Lv, Hai tao; Zhang, Ai hua; Sun, Hui; Yan, Guang li; Han, Ying; Wu, Xiu hong; Wang, Xi jun

    2013-11-01

    Liuwei Dihuang Wan (LDW), a classic Chinese medicinal formula, has been used to improve or restore declined functions related to aging and geriatric diseases, such as impaired mobility, vision, hearing, cognition, and memory. It has attracted increasing attention as one of the most popular and valuable herbal medicines. However, the systematic analysis of the chemical constituents of LDW is difficult and thus has not been well established. In this paper, a rapid, sensitive, and reliable ultra-performance LC with ESI quadrupole TOF high-definition MS method with automated MetaboLynx analysis in positive and negative ion mode was established to characterize the chemical constituents of LDW. The analysis was performed on a Waters UPLC™ HSS T3 using a gradient elution system. MS/MS fragmentation behavior was proposed for aiding the structural identification of the components. Under the optimized conditions, a total of 50 peaks were tentatively characterized by comparing the retention time and MS data. It is concluded that a rapid and robust platform based on ultra-performance LC with ESI quadrupole TOF high-definition MS has been successfully developed for globally identifying multiple constituents of traditional Chinese medicine prescriptions. This is the first report on the systematic analysis of the chemical constituents of LDW. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Time-of-flight spectrometers

    International Nuclear Information System (INIS)

    Carrico, J.P.

    1976-01-01

    The flight time of an ion in an inhomogeneous, oscillatory electric field (IOFE) is an m/e-dependent property of this field and is independent of the initial position and velocity. The d.c. component of the equation of motion for an ion in the IOFE describes a harmonic oscillation of constant period. When ions oscillate for many periods with one species overtaking another the motion may no longer be truly periodic although the resulting period or 'quasi-period' still remains independent of the initial conditions. This period or 'quasi-period' is used in the time-of-flight mass spectrometer described. The principle of operation is also described and both analytical and experimental results are reported. (B.D.)

  8. The ANTARES recoil time-of-flight spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Martin, J W; Russell, G J [New South Wales Univ., Kensington, NSW (Australia); Cohen, D D; Dytlewski, N [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1997-12-31

    The Australian National Tandem for Applied Research (ANTARES), is a 8MV FN tandem particle accelerator at the Australian Nuclear Science and Technology Organisation. Research on the accelerator is divided between two groups, Accelerator Mass Spectrometry (AMS) and lon Beam Analysis (IBA). The IBA group carries out a range of research projects from nuclear physics to materials characterisation. The major IBA project on the accelerator is a recoil time-of-flight spectrometer which consists of two electrostatic time pulse generators and an ion-implanted surface barrier detector. The spectrometer is ideally suited to the profiling of layered multi-element materials, and has been used to characterise materials such as metal-germanides, optoelectronics, superconductors and catalytic converters. This paper will describe the time-of-flight system as well as some recent materials characterisation results. 1 refs., 3 figs.

  9. The ANTARES recoil time-of-flight spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Martin, J.W.; Russell, G.J. [New South Wales Univ., Kensington, NSW (Australia); Cohen, D.D.; Dytlewski, N. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    The Australian National Tandem for Applied Research (ANTARES), is a 8MV FN tandem particle accelerator at the Australian Nuclear Science and Technology Organisation. Research on the accelerator is divided between two groups, Accelerator Mass Spectrometry (AMS) and lon Beam Analysis (IBA). The IBA group carries out a range of research projects from nuclear physics to materials characterisation. The major IBA project on the accelerator is a recoil time-of-flight spectrometer which consists of two electrostatic time pulse generators and an ion-implanted surface barrier detector. The spectrometer is ideally suited to the profiling of layered multi-element materials, and has been used to characterise materials such as metal-germanides, optoelectronics, superconductors and catalytic converters. This paper will describe the time-of-flight system as well as some recent materials characterisation results. 1 refs., 3 figs.

  10. Electrostatic design and beam transport for a folded tandem electrostatic quadrupole accelerator facility for accelerator-based boron neutron capture therapy

    International Nuclear Information System (INIS)

    Thatar Vento, V.; Bergueiro, J.; Cartelli, D.; Valda, A.A.; Kreiner, A.J.

    2011-01-01

    Within the frame of an ongoing project to develop a folded Tandem-Electrostatic-Quadrupole (TESQ) accelerator facility for Accelerator-Based Boron Neutron Capture Therapy (AB-BNCT), we discuss here the electrostatic design of the machine, including the accelerator tubes with electrostatic quadrupoles and the simulations for the transport and acceleration of a high intensity beam.

  11. Atmospheric pressure solid analysis probe coupled to quadrupole-time of flight mass spectrometry as a tool for screening and semi-quantitative approach of polycyclic aromatic hydrocarbons, nitro-polycyclic aromatic hydrocarbons and oxo-polycyclic aromatic hydrocarbons in complex matrices.

    Science.gov (United States)

    Carrizo, Daniel; Domeño, Celia; Nerín, Isabel; Alfaro, Pilar; Nerín, Cristina

    2015-01-01

    A new screening and semi-quantitative approach has been developed for direct analysis of polycyclic aromatic hydrocarbons (PAHs) and their nitro and oxo derivatives in environmental and biological matrices using atmospheric pressure solid analysis probe (ASAP) quadrupole-time of flight mass spectrometry (Q-TOF-MS). The instrumental parameters were optimized for the analysis of all these compounds, without previous sample treatment, in soil, motor oil, atmospheric particles (ashes) and biological samples such as urine and saliva of smokers and non-smokers. Ion source parameters in the MS were found to be the key parameters, with little variation within PAHs families. The optimized corona current was 4 µA, sample cone voltage 80 V for PAHs, nitro-PAHs and oxo-PAHs, while the desolvation temperatures varied from 300°C to 500°C. The analytical method performance was checked using a certified reference material. Two deuterated compounds were used as internal standards for semi-quantitative purposes together with the pure individual standard for each compound and the corresponding calibration plot. The compounds nitro PAH 9-nitroanthracene and oxo-PAH 1,4-naphthalenedione, were found in saliva and urine in a range below 1 µg/g while the range of PAHs in these samples was below 2 µg/g. Environmental samples provided higher concentration of all pollutants than urine and saliva. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Development of a Tandem-ElectroStatic-Quadrupole accelerator facility for Boron Neutron Capture Therapy (BNCT)

    International Nuclear Information System (INIS)

    Kreiner, A.J.; Thatar Vento, V.; Levinas, P.; Bergueiro, J.; Burlon, A.A.; Di Paolo, H.; Kesque, J.M.; Valda, A.A.; Debray, M.E.; Somacal, H.R.; Minsky, D.M.; Estrada, L.; Hazarabedian, A.; Johann, F.; Suarez Sandin, J.C.; Castell, W.; Davidson, J.; Davidson, M.; Repetto, M.; Obligado, M.; Nery, J.P.; Huck, H.; Igarzabal, M.; Fernandez Salares, A.

    2008-01-01

    There is a generalized perception that the availability of suitable particle accelerators installed in hospitals, as neutron sources, may be crucial for the advancement of Boron Neutron Capture Therapy (BNCT). An ongoing project to develop a Tandem-ElectroStatic-Quadrupole (TESQ) accelerator facility for Accelerator-Based (AB)-BNCT is described here. The project goal is a machine capable of delivering 30 mA of 2.4-2.5 MeV protons to be used in conjunction with a neutron production target based on the 7 Li(p,n) 7 Be reaction slightly beyond its resonance at 2.25 MeV. A folded tandem, with 1.20-1.25 MV terminal voltage, combined with an ESQ chain is being designed and constructed. This machine is conceptually shown to be capable of accelerating a 30 mA proton beam to 2.5 MeV. These are the specifications needed to produce sufficiently intense and clean epithermal neutron beams, based on the 7 Li(p,n) 7 Be reaction, to perform BNCT treatment for deep-seated tumors in less than an hour. This electrostatic machine is one of the technologically simplest and cheapest solutions for optimized AB-BNCT. At present there is no BNCT facility in the world with the characteristics presented in this work. For the accelerator, results on its design, construction and beam transport calculations are discussed. Taking into account the peculiarities of the expected irradiation field, the project also considers a specific study of the treatment room. This study aims at the design of the treatment room emphasizing aspects related to patient, personnel and public radiation protection; dose monitoring; patient positioning and room construction. The design considers both thermal (for the treatment of shallow tumors) and epithermal (for deep-seated tumors) neutron beams entering the room through a port connected to the accelerator via a moderation and neutron beam shaping assembly. Preliminary results of dose calculations for the treatment room design, using the MCNP program, are presented

  13. Development of a tandem-electrostatic-quadrupole accelerator facility for BNCT

    International Nuclear Information System (INIS)

    Kreiner, A.J.; Thatar Vento, V.; Levinas, P.; Bergueiro, J.; Di Paolo, H.; Burlon, A.A.; Kesque, J.M.; Valda, A.A.; Debray, M.E.; Somacal, H.R.; Minsky, D.M.

    2009-01-01

    In this work we describe the present status of an ongoing project to develop a tandem-electrostatic-quadrupole (TESQ) accelerator facility for accelerator-based (AB) BNCT at the Atomic Energy Commission of Argentina in Buenos Aires. The project final goal is a machine capable of delivering 30 mA of 2.4 MeV protons to be used in conjunction with a neutron production target based on the 7 Li(p,n) 7 Be reaction slightly beyond its resonance at 2.25 MeV. These are the specifications needed to produce sufficiently intense and clean epithermal neutron beams, based on the 7 Li(p,n) 7 Be reaction, to perform BNCT treatment for deep-seated tumors in less than an hour. An electrostatic machine is the technologically simplest and cheapest solution for optimized AB-BNCT. The machine being designed and constructed is a folded TESQ with a high-voltage terminal at 1.2 MV intended to work in air. Such a machine is conceptually shown to be capable of transporting and accelerating a 30 mA proton beam to 2.4 MeV. The general geometric layout, its associated electrostatic fields, and the acceleration tube are simulated using a 3D finite element procedure. The design and construction of the ESQ modules is discussed and their electrostatic fields are investigated. Beam transport calculations through the accelerator are briefly mentioned. Likewise, work related to neutron production targets, strippers, beam shaping assembly and patient treatment room is briefly described.

  14. Development of a tandem-electrostatic-quadrupole accelerator facility for BNCT.

    Science.gov (United States)

    Kreiner, A J; Thatar Vento, V; Levinas, P; Bergueiro, J; Di Paolo, H; Burlon, A A; Kesque, J M; Valda, A A; Debray, M E; Somacal, H R; Minsky, D M; Estrada, L; Hazarabedian, A; Johann, F; Suarez Sandin, J C; Castell, W; Davidson, J; Davidson, M; Giboudot, Y; Repetto, M; Obligado, M; Nery, J P; Huck, H; Igarzabal, M; Fernandez Salares, A

    2009-07-01

    In this work we describe the present status of an ongoing project to develop a tandem-electrostatic-quadrupole (TESQ) accelerator facility for accelerator-based (AB) BNCT at the Atomic Energy Commission of Argentina in Buenos Aires. The project final goal is a machine capable of delivering 30 mA of 2.4 MeV protons to be used in conjunction with a neutron production target based on the (7)Li(p,n)(7)Be reaction slightly beyond its resonance at 2.25 MeV. These are the specifications needed to produce sufficiently intense and clean epithermal neutron beams, based on the (7)Li(p,n)(7)Be reaction, to perform BNCT treatment for deep-seated tumors in less than an hour. An electrostatic machine is the technologically simplest and cheapest solution for optimized AB-BNCT. The machine being designed and constructed is a folded TESQ with a high-voltage terminal at 1.2 MV intended to work in air. Such a machine is conceptually shown to be capable of transporting and accelerating a 30 mA proton beam to 2.4 MeV. The general geometric layout, its associated electrostatic fields, and the acceleration tube are simulated using a 3D finite element procedure. The design and construction of the ESQ modules is discussed and their electrostatic fields are investigated. Beam transport calculations through the accelerator are briefly mentioned. Likewise, work related to neutron production targets, strippers, beam shaping assembly and patient treatment room is briefly described.

  15. Qualitative and quantitative analysis of the saponins in Panax notoginseng leaves using ultra-performance liquid chromatography coupled with time-of-flight tandem mass spectrometry and high performance liquid chromatography coupled with UV detector.

    Science.gov (United States)

    Liu, Fang; Ma, Ni; He, Chengwei; Hu, Yuanjia; Li, Peng; Chen, Meiwan; Su, Huanxing; Wan, Jian-Bo

    2018-04-01

    Panax notoginseng leaves (PNL) exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS) and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL-ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd-were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of 35°C. This developed HPLC-UV method provides an adequate linearity ( r 2  > 0.999), repeatability (relative standard deviation, RSD PNL. These findings are beneficial to the quality control of PNL and its relevant products.

  16. High-Performance Liquid Chromatography with Diode Array Detector and Electrospray Ionization Ion Trap Time-of-Flight Tandem Mass Spectrometry to Evaluate Ginseng Roots and Rhizomes from Different Regions.

    Science.gov (United States)

    Wang, Hong-Ping; Zhang, You-Bo; Yang, Xiu-Wei; Yang, Xin-Bao; Xu, Wei; Xu, Feng; Cai, Shao-Qing; Wang, Ying-Ping; Xu, Yong-Hua; Zhang, Lian-Xue

    2016-05-09

    Ginseng, Panax ginseng C. A. Meyer, is an industrial crop in China and Korea. The functional components in ginseng roots and rhizomes are characteristic ginsenosides. This work developed a new high-performance liquid chromatography coupled with electrospray ionization ion trap time-of-flight multistage mass spectrometry (LC-ESI-IT-TOF-MS(n)) method to identify the triterpenoids. Sixty compounds (1-60) including 58 triterpenoids were identified from the ginseng cultivated in China. Substances 1, 2, 7, 15-20, 35, 39, 45-47, 49, 55-57, 59, and 60 were identified for the first time. To evaluate the quality of ginseng cultivated in Northeast China, this paper developed a practical liquid chromatography-diode array detection (LC-DAD) method to simultaneously quantify 14 interesting ginsenosides in ginseng collected from 66 different producing areas for the first time. The results showed the quality of ginseng roots and rhizomes from different sources was different due to growing environment, cultivation technology, and so on. The developed LC-ESI-IT-TOF-MS(n) method can be used to identify many more ginsenosides and the LC-DAD method can be used not only to assess the quality of ginseng, but also to optimize the cultivation conditions for the production of ginsenosides.

  17. Doppler time-of-flight imaging

    KAUST Repository

    Heidrich, Wolfgang; Heide, Felix; Wetzstein, Gordon; Hullin, Matthias

    2017-01-01

    Systems and methods for imaging object velocity are provided. In an embodiment, at least one Time-of-Flight camera is used to capture a signal representative of an object in motion over an exposure time. Illumination and modulation frequency

  18. Qualitative and quantitative analysis of the saponins in Panax notoginseng leaves using ultra-performance liquid chromatography coupled with time-of-flight tandem mass spectrometry and high performance liquid chromatography coupled with UV detector

    Directory of Open Access Journals (Sweden)

    Fang Liu

    2018-04-01

    Full Text Available Background: Panax notoginseng leaves (PNL exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Methods: Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Results: Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL—ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd—were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of 35°C. This developed HPLC-UV method provides an adequate linearity (r2>0.999, repeatability (relative standard deviation, RSD < 2.98%, and inter- and intraday variations (RSD < 4.40% with recovery (98.7–106.1% of seven saponins concerned. This validated method was also conducted to determine seven components in 10 batches of PNL. Conclusion: These findings are beneficial to the quality control of PNL and its relevant products. Keywords: ginsenoside transformation, notoginsenoside Fd, notoginsenoside Fe, Panax notoginseng leaves, UPLC/Q-TOF MS

  19. Principles of time-of-flight tomography

    International Nuclear Information System (INIS)

    Campagnolo, R.; Garderet, P.; Lecomte, J.L.; Bouvier, A.; Darier, P.; Soussaline, F.

    1983-03-01

    After a short introduction to the physics of time-of-flight positron tomography, the various aspects of this technique are presented. The characteristics including data acquisition and image reconstruction system of a positron tomograph (TTV01) which uses time-of-flight information, are described. The preliminary results obtained with TTV01, such as resolution and sensitivity, as well as phantom images, are presented [fr

  20. Matrix interference evaluation employing GC and LC coupled to triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Uclés, S; Lozano, A; Sosa, A; Parrilla Vázquez, P; Valverde, A; Fernández-Alba, A R

    2017-11-01

    Gas and liquid chromatography coupled to triple quadrupole tandem mass spectrometry are currently the most powerful tools employed for the routine analysis of pesticide residues in food control laboratories. However, whatever the multiresidue extraction method, there will be a residual matrix effect making it difficult to identify/quantify some specific compounds in certain cases. Two main effects stand out: (i) co-elution with isobaric matrix interferents, which can be a major drawback for unequivocal identification, and therefore false negative detections, and (ii) signal suppression/enhancement, commonly called the "matrix effect", which may cause serious problems including inaccurate quantitation, low analyte detectability and increased method uncertainty. The aim of this analytical study is to provide a framework for evaluating the maximum expected errors associated with the matrix effects. The worst-case study contrived to give an estimation of the extreme errors caused by matrix effects when extraction/determination protocols are applied in routine multiresidue analysis. Twenty-five different blank matrices extracted with the four most common extraction methods used in routine analysis (citrate QuEChERS with/without PSA clean-up, ethyl acetate and the Dutch mini-Luke "NL" methods) were evaluated by both GC-QqQ-MS/MS and LC-QqQ-MS/MS. The results showed that the presence of matrix compounds with isobaric transitions to target pesticides was higher in GC than under LC in the experimental conditions tested. In a second study, the number of "potential" false negatives was evaluated. For that, ten matrices with higher percentages of natural interfering components were checked. Additionally, the results showed that for more than 90% of the cases, pesticide quantification was not affected by matrix-matched standard calibration when an interferent was kept constant along the calibration curve. The error in quantification depended on the concentration level. In a

  1. Electrostatic design and beam transport for a folded tandem electrostatic quadrupole accelerator facility for accelerator-based boron neutron capture therapy.

    Science.gov (United States)

    Vento, V Thatar; Bergueiro, J; Cartelli, D; Valda, A A; Kreiner, A J

    2011-12-01

    Within the frame of an ongoing project to develop a folded Tandem-Electrostatic-Quadrupole (TESQ) accelerator facility for Accelerator-Based Boron Neutron Capture Therapy (AB-BNCT), we discuss here the electrostatic design of the machine, including the accelerator tubes with electrostatic quadrupoles and the simulations for the transport and acceleration of a high intensity beam. Copyright © 2011 Elsevier Ltd. All rights reserved.

  2. Complete Analysis of a Biologically Active Tetrapeptide: A Project Utilizing Thin-Layer Chromatography and Tandem Quadrupole Mass Spectrometry

    Science.gov (United States)

    Lefevre, Joseph W.; Dodsworth, David W.

    2000-04-01

    The biologically active tetrapeptide d-Ala-Gly-l-Phe-d-Leu ([des-Tyr1-d-Ala2-d-Leu5]enkephalin) was analyzed for its amino acid content and stereochemistry by normal and reversed-phase thin-layer chromatography (TLC), and its sequence was determined by tandem quadrupole mass spectrometry. The project involved sequential N-dansylation of a portion of the tetrapeptide, hydrolysis, isolation, and identification of the N-terminal amino acid as dansyl-alanine by comparison with standards using normal-phase TLC. A second portion of the tetrapeptide was hydrolyzed and the resulting four free amino acids were converted to their corresponding dansyl derivatives and purified by preparative normal-phase TLC. The three dansyl amino acids not identified previously were identified by TLC. The stereochemistry of each was determined by comparison with dansyl-dl-amino acid standards using reversed-phase TLC in the presence of ß-cyclodextrin, a chiral mobile phase additive. Finally, the correct amino acid sequence was determined by tandem quadrupole mass spectrometry. This project gives students valuable experience in microscale synthesis, both normal and reversed-phase TLC, stereochemical analysis, and mass spectrometry.

  3. Thin Time-Of-Flight PET project

    CERN Multimedia

    The pre-R&D aims at designing and producing a compact and thin Time-Of-Flight PET detector device with depth of interaction measurement capability, which employs layered silicon sensors as active material, with a readout consisting of a new generation of very-low noise and very fast electronics based on SiGe Heterojunction Bipolar Transistors (HBT) components.

  4. Ultra-high performance liquid chromatography coupled with photo-diode array and quadrupole/time-of-flight mass spectrometry based chemical profiling approach to evaluate the influence of preparation methods on the holistic quality of Qiong-Yu-Gao, a traditional complex herbal medicine.

    Science.gov (United States)

    Xu, Jin-Di; Mao, Qian; Shen, Hong; Zhu, Ling-Ying; Li, Song-Lin; Yan, Ru

    2013-08-23

    Qiong-Yu-Gao (QYG), consisting of Rehmanniae Radix (RR), Poriae (PO) and Ginseng Radix (GR), is a commonly used tonic traditional complex herbal medicine (CHM). So far, three different methods have been documented for preparation of QYG, i.e. method 1 (M1): mixing powders of GR and PO with decoction of RR; method 2 (M2): combining the decoction of RR and PO with the decoction of GR; method 3 (M3): decocting the mixture of RR, GR and PO. In present study, an ultra-high performance liquid chromatography coupled with photo-diode array and quadrupole/time-of-flight mass spectrometry (UHPLC-PDA-QTOF-MS/MS) based chemical profiling approach was developed to investigate the influence of the three preparation methods on the holistic quality of QYG. All detected peaks were unambiguously identified by comparing UV spectra, accurate mass data/characteristic mass fragments and retention times with those of reference compounds, and/or tentatively assigned by matching empirical molecular formula with that of known compounds, and/or elucidating quasi-molecular ions and fragment ions referring to information available in literature. A total of 103 components, mainly belonging to ginsenosides, phenethylalcohol glycosides, iridoid glycosides and triterpenoid acids, were identified, of which 5 degraded ginsenosides were putatively determined to be newly generated during preparation procedures of QYG samples. Triterpenoid acids and malonyl-ginsenosides were detected only in M1 samples, while degraded ginsenosides were merely detectable in M2/M3 samples. The possible reasons for the difference among chemical profiles of QYG samples prepared with three methods were also discussed. It could be concluded that preparation method do significantly affect the holistic quality of QYG. The influence of the altered chemical profiles on the bioactivity of QYG needs further investigation. The present study demonstrated that UHPLC-PDA-QTOF-MS/MS based chemical profiling approach is efficient and

  5. The ARGUS time-of-flight system

    International Nuclear Information System (INIS)

    Heller, R.; Klinger, T.; Salomon, R.; Schubert, K.R.; Stiewe, J.; Waldi, R.; Weseler, S.

    1985-01-01

    The time-of-flight system of the ARGUS detector at the DORIS e + e - storage ring consists of 64 barrel scintillation counters covering 75% of 4π, and 2x48 end cap counters, covering 17% of 4π. The barrel counters are viewed by two phototubes each, while the end cap counters have one tube only. The time-of-flight system serves as a part of the fast trigger and identifies charged particles. The time resolution achieved during the first year of ARGUS operation is 210 ps for Bhabhas (which are used for the off-line monitoring of the system), and 220 ps for hadrons, both in barrel and end cap counters. This converts into a three standard deviation mass separation up to 700 MeV/c between pions and kaons and 1200 MeV/c between kaons and protons. Electrons can be separated from heavier particles up to 230 MeV/c. (orig.)

  6. SHMS Hodoscopes and Time of Flight System

    Science.gov (United States)

    Craycraft, Kayla; Malace, Simona

    2017-09-01

    As part of the Thomas Jefferson National Accelerator Facility's (Jefferson Lab) upgrade from 6 GeV to 12 GeV, a new magnetic focusing spectrometer, the Super High Momentum Spectrometer (SHMS), was installed in experimental Hall C. The detector stack consists of horizontal drift chambers for tracking, gas Cerenkov and Aerogel detectors and a lead glass calorimeter for particle identification. A hodoscope system consisting of three planes of scintillator detectors (constructed by James Madison University) and one plane of quartz bars (built by North Carolina A&T State University) is used for triggering and time of flight measurements. This presentation consists of discussion of the installation, calibration, and characterization of the detectors used in this Time of Flight system. James Madison University, North Carolina A&T State University.

  7. Accelerator-Based Boron Neutron Capture Therapy and the Development of a Dedicated Tandem-Electrostatic-Quadrupole

    International Nuclear Information System (INIS)

    Kreiner, A. J.; Di Paolo, H.; Burlon, A. A.; Valda, A. A.; Debray, M. E.; Somacal, H. R.; Minsky, D. M.; Kesque, J. M.; Giboudot, Y.; Levinas, P.; Fraiman, M.; Romeo, V.

    2007-01-01

    There is a generalized perception that the availability of suitable particle accelerators installed in hospitals, as neutron sources, may be crucial for the advancement of Boron Neutron Capture Therapy (BNCT). Progress on an ongoing project to develop a Tandem-ElectroStatic-Quadrupole (TESQ) accelerator for Accelerator-Based (AB)-BNCT is described here. The project goal is a machine capable of delivering 30 mA of 2.5 MeV protons to be used in conjunction with a neutron production target based on the 7 Li(p,n) 7 Be reaction slightly beyond its resonance at 2.25 MeV. A folded tandem, with 1.25 MV terminal voltage, combined with an ESQ chain is being designed and constructed. A 30 mA proton beam of 2.5 MeV are the specifications needed to produce sufficiently intense and clean epithermal neutron beams, based on the 7 Li(p,n) 7 Be reaction, to perform BNCT treatment for deep-seated tumors in less than an hour. The first design and construction of an ESQ module is discussed and its electrostatic fields are investigated theoretically and experimentally. Also new beam transport calculations through the accelerator are presented

  8. Liquid chromatography coupled to quadrupole-time of flight tandem mass spectrometry based quantitative structure-retention relationships of amino acid analogues derivatized via n-propyl chloroformate mediated reaction.

    Science.gov (United States)

    Kritikos, Nikolaos; Tsantili-Kakoulidou, Anna; Loukas, Yannis L; Dotsikas, Yannis

    2015-07-17

    In the current study, quantitative structure-retention relationships (QSRR) were constructed based on data obtained by a LC-(ESI)-QTOF-MS/MS method for the determination of amino acid analogues, following their derivatization via chloroformate esters. Molecules were derivatized via n-propyl chloroformate/n-propanol mediated reaction. Derivatives were acquired through a liquid-liquid extraction procedure. Chromatographic separation is based on gradient elution using methanol/water mixtures from a 70/30% composition to an 85/15% final one, maintaining a constant rate of change. The group of examined molecules was diverse, including mainly α-amino acids, yet also β- and γ-amino acids, γ-amino acid analogues, decarboxylated and phosphorylated analogues and dipeptides. Projection to latent structures (PLS) method was selected for the formation of QSRRs, resulting in a total of three PLS models with high cross-validated coefficients of determination Q(2)Y. For this reason, molecular structures were previously described through the use of descriptors. Through stratified random sampling procedures, 57 compounds were split to a training set and a test set. Model creation was based on multiple criteria including principal component significance and eigenvalue, variable importance, form of residuals, etc. Validation was based on statistical metrics Rpred(2),QextF2(2),QextF3(2) for the test set and Roy's metrics rm(Av)(2) and rm(δ)(2), assessing both predictive stability and internal validity. Based on aforementioned models, simplified equivalent were then created using a multi-linear regression (MLR) method. MLR models were also validated with the same metrics. The suggested models are considered useful for the estimation of retention times of amino acid analogues for a series of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Time-of-flight mass spectrometer

    International Nuclear Information System (INIS)

    Ivanov, M.A.; Kozlov, B.N.; Mamyrin, B.A.; Shmikk, D.V.; Shebelin, V.G.

    1981-01-01

    A time-of-flight mass spectrometer containing a pulsed ion source with an electron gun and two electrodes limiting ionization range, drift space and ion acceptor, is described. To expand functional possibilities, a slot collimator of the gas stream, two quantum generators and two diaphragms for the inlet of quantum generator radiation located on both sides of the ion source, are introduced in the ion source. The above invention enables to study details of the complex interaction process of laser radiation with molecules of the gas stream, which is actual for laser isotope separation

  10. Doppler time-of-flight imaging

    KAUST Repository

    Heide, Felix

    2015-07-30

    Over the last few years, depth cameras have become increasingly popular for a range of applications, including human-computer interaction and gaming, augmented reality, machine vision, and medical imaging. Many of the commercially-available devices use the time-of-flight principle, where active illumination is temporally coded and analyzed on the camera to estimate a per-pixel depth map of the scene. In this paper, we propose a fundamentally new imaging modality for all time-of-flight (ToF) cameras: per-pixel velocity measurement. The proposed technique exploits the Doppler effect of objects in motion, which shifts the temporal frequency of the illumination before it reaches the camera. Using carefully coded illumination and modulation frequencies of the ToF camera, object velocities directly map to measured pixel intensities. We show that a slight modification of our imaging system allows for color, depth, and velocity information to be captured simultaneously. Combining the optical flow computed on the RGB frames with the measured metric axial velocity allows us to further estimate the full 3D metric velocity field of the scene. We believe that the proposed technique has applications in many computer graphics and vision problems, for example motion tracking, segmentation, recognition, and motion deblurring.

  11. The TORCH time-of-flight detector

    Energy Technology Data Exchange (ETDEWEB)

    Harnew, N., E-mail: Neville.Harnew@physics.ox.ac.uk [University of Oxford, Denys Wilkinson Building, 1 Keble Road, Oxford OX1 3RH (United Kingdom); Brook, N. [University College London, Department of Physics & Astronomy, Gower Street, London WC1E 6BT (United Kingdom); Castillo García, L. [CERN, PH Department, CH-1211 Geneva 23 (Switzerland); Laboratory for High Energy Physics, Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne (Switzerland); Cussans, D. [H.H. Wills Physics Laboratory, University of Bristol, Bristol BS8 1TL (United Kingdom); Föhl, K.; Forty, R.; Frei, C. [CERN, PH Department, CH-1211 Geneva 23 (Switzerland); Gao, R. [University of Oxford, Denys Wilkinson Building, 1 Keble Road, Oxford OX1 3RH (United Kingdom); Gys, T.; Piedigrossi, D. [CERN, PH Department, CH-1211 Geneva 23 (Switzerland); Rademacker, J.; Ros Garcia, A.; Dijk, M. van [H.H. Wills Physics Laboratory, University of Bristol, Bristol BS8 1TL (United Kingdom)

    2016-07-11

    The TORCH time-of-flight detector is being developed to provide particle identification between 2 and 10 GeV/c momentum over a flight distance of 10 m. TORCH is designed for large-area coverage, up to 30 m{sup 2}, and has a DIRC-like construction. The goal is to achieve a 15 ps time-of-flight resolution per incident particle by combining arrival times from multiple Cherenkov photons produced within quartz radiator plates of 10 mm thickness. A four-year R&D programme is underway with an industrial partner (Photek, UK) to produce 53×53 mm{sup 2} Micro-Channel Plate (MCP) detectors for the TORCH application. The MCP-PMT will provide a timing accuracy of 40 ps per photon and it will have a lifetime of up to at least 5 Ccm{sup −2} of integrated anode charge by utilizing an Atomic Layer Deposition (ALD) coating. The MCP will be read out using charge division with customised electronics incorporating the NINO chipset. Laboratory results on prototype MCPs are presented. The construction of a prototype TORCH module and its simulated performance are also described.

  12. Doppler time-of-flight imaging

    KAUST Repository

    Heidrich, Wolfgang

    2017-02-16

    Systems and methods for imaging object velocity are provided. In an embodiment, at least one Time-of-Flight camera is used to capture a signal representative of an object in motion over an exposure time. Illumination and modulation frequency of the captured motion are coded within the exposure time. A change of illumination frequency is mapped to measured pixel intensities of the captured motion within the exposure time, and information about a Doppler shift in the illumination frequency is extracted to obtain a measurement of instantaneous per pixel velocity of the object in motion. The radial velocity information of the object in motion can be simultaneously captured for each pixel captured within the exposure time. In one or more aspects, the illumination frequency can be coded orthogonal to the modulation frequency of the captured motion. The change of illumination frequency can correspond to radial object velocity.

  13. Time of flight spectroscopy with muonic hydrogen

    International Nuclear Information System (INIS)

    Marshall, G.M.; Bailey, J.M.; Beer, G.A.

    1993-01-01

    Time of flight techniques coupled with muonic deuterium and tritium atoms in vacuum can be used to measure parameters important in the understanding of muon catalyzed fusion interactions. Muonic deuterium atomic beams with energy of order 1 eV have been produced via transfer and emission from solid hydrogen containing small deuterium concentrations. Measurements of energy loss in pure deuterium are presented which test calculations of σ μd+D . Muonic tritium beams should be produced in a similar way, with an energy distribution which overlaps the predicted muonic molecular (dμt) formation resonances. The existence of resonances is crucial for high cycling rates in muon catalyzed fusion, but direct experimental verification of strengths and energies is not yet possible by other means. Results of simulations demonstrate how the resonance structure might be confirmed

  14. Pesticide residues determination in Polish organic crops in 2007-2010 applying gas chromatography-tandem quadrupole mass spectrometry.

    Science.gov (United States)

    Walorczyk, Stanisław; Drożdżyński, Dariusz; Kowalska, Jolanta; Remlein-Starosta, Dorota; Ziółkowski, Andrzej; Przewoźniak, Monika; Gnusowski, Bogusław

    2013-08-15

    A sensitive, accurate and reliable multiresidue method based on the application of gas chromatography-tandem quadrupole mass spectrometry (GC-QqQ-MS/MS) has been established for screening, identification and quantification of a large number of pesticide residues in produce. The method was accredited in compliance with PN-EN ISO/IEC 17025:2005 standard and it was operated under flexible scope as PB-11 method. The flexible scope of accreditation allowed for minor modifications and extension of the analytical scope while using the same analytical technique. During the years 2007-2010, the method was used for the purpose of verification of organic crop production by multiresidue analysis for the presence of pesticides. A total of 528 samples of differing matrices such as fruits, vegetables, cereals, plant leaves and other green parts were analysed, of which 4.4% samples contained pesticide residues above the threshold value of 0.01 mg/kg. A total of 20 different pesticide residues were determined in the samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. [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.

  16. 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.

  17. Characterizing Scintillator Response with Neutron Time-of-Flight

    Science.gov (United States)

    Palmisano, Kevin; Visca, Hannah; Caves, Louis; Wilkinson, Corey; McClow, Hannah; Padalino, Stephen; Forrest, Chad; Katz, Joe; Sangster, Craig; Regan, Sean

    2017-10-01

    Neutron scintillator diagnostics for ICF can be characterized using the neutron time-of-flight (nTOF) line on Geneseo's 1.7 MV Tandem Pelletron Accelerator. Neutron signals can be differentiated from gamma signals by employing a coincidence method called the associated particle technique (APT). In this measurement, a 2.1 MeV beam of deuterons incident on a deuterated polyethylene target produces neutrons via the d(d,n)3He reaction. A BC-412 plastic scintillator, placed at a scattering angle of 152º, detects 1.76 MeV neutrons in coincidence with the 2.56 MeV 3He ions at an associated angle of 10º. The APT is used to identify the 1.76 MeV neutron while the nTOF line determines its energy. By gating only mono-energetic neutrons, the instrument response function of the scintillator can be determined free from background scattered neutrons and gamma rays. Funded in part by a Grant from the DOE, through the Laboratory for Laser Energetics.

  18. A qualitative study of amlodipine and its related compounds by electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Gibbons, John; Pugh, Jonathan; Dimopoulos-Italiano, Gina; Pike, Richard

    2006-01-01

    A comprehensive structural analysis of amlodipine and certain related compounds was performed by electrospray ionization tandem mass spectrometry. Triple quadrupole and quadrupole time-of-flight instruments were used to provide collision-induced dissociation and accurate mass measurement for selected product and second-generation product ions. A unique ion rearrangement was observed, which was found to be characteristic of certain dihydropyridines. This study provides a fundamental understanding of the fragmentation of these compounds. The structural elucidation of an unknown impurity is presented as an example. Copyright (c) 2006 John Wiley & Sons, Ltd.

  19. Development of high intensity ion sources for a Tandem-Electrostatic-Quadrupole facility for Accelerator-Based Boron Neutron Capture Therapy

    International Nuclear Information System (INIS)

    Bergueiro, J.; Igarzabal, M.; Suarez Sandin, J.C.; Somacal, H.R.; Thatar Vento, V.; Huck, H.; Valda, A.A.; Repetto, M.

    2011-01-01

    Several ion sources have been developed and an ion source test stand has been mounted for the first stage of a Tandem-Electrostatic-Quadrupole facility For Accelerator-Based Boron Neutron Capture Therapy. A first source, designed, fabricated and tested is a dual chamber, filament driven and magnetically compressed volume plasma proton ion source. A 4 mA beam has been accelerated and transported into the suppressed Faraday cup. Extensive simulations of the sources have been performed using both 2D and 3D self-consistent codes.

  20. Development of high intensity ion sources for a Tandem-Electrostatic-Quadrupole facility for Accelerator-Based Boron Neutron Capture Therapy

    Energy Technology Data Exchange (ETDEWEB)

    Bergueiro, J. [Gerencia de Investigacion y Aplicaciones, Comision Nacional de Energia Atomica (Argentina)] [CONICET, Buenos Aires (Argentina); Igarzabal, M.; Suarez Sandin, J.C. [Gerencia de Investigacion y Aplicaciones, Comision Nacional de Energia Atomica (Argentina); Somacal, H.R. [Gerencia de Investigacion y Aplicaciones, Comision Nacional de Energia Atomica (Argentina)] [Escuela de Ciencia y Tecnologia, Universidad Nacional de San Martin (Argentina); Thatar Vento, V. [Gerencia de Investigacion y Aplicaciones, Comision Nacional de Energia Atomica (Argentina)] [CONICET, Buenos Aires (Argentina); Huck, H.; Valda, A.A. [Gerencia de Investigacion y Aplicaciones, Comision Nacional de Energia Atomica (Argentina)] [Escuela de Ciencia y Tecnologia, Universidad Nacional de San Martin (Argentina); Repetto, M. [Gerencia de Investigacion y Aplicaciones, Comision Nacional de Energia Atomica (Argentina)

    2011-12-15

    Several ion sources have been developed and an ion source test stand has been mounted for the first stage of a Tandem-Electrostatic-Quadrupole facility For Accelerator-Based Boron Neutron Capture Therapy. A first source, designed, fabricated and tested is a dual chamber, filament driven and magnetically compressed volume plasma proton ion source. A 4 mA beam has been accelerated and transported into the suppressed Faraday cup. Extensive simulations of the sources have been performed using both 2D and 3D self-consistent codes.

  1. Development of high intensity ion sources for a Tandem-Electrostatic-Quadrupole facility for Accelerator-Based Boron Neutron Capture Therapy.

    Science.gov (United States)

    Bergueiro, J; Igarzabal, M; Sandin, J C Suarez; Somacal, H R; Vento, V Thatar; Huck, H; Valda, A A; Repetto, M; Kreiner, A J

    2011-12-01

    Several ion sources have been developed and an ion source test stand has been mounted for the first stage of a Tandem-Electrostatic-Quadrupole facility For Accelerator-Based Boron Neutron Capture Therapy. A first source, designed, fabricated and tested is a dual chamber, filament driven and magnetically compressed volume plasma proton ion source. A 4 mA beam has been accelerated and transported into the suppressed Faraday cup. Extensive simulations of the sources have been performed using both 2D and 3D self-consistent codes. Copyright © 2011 Elsevier Ltd. All rights reserved.

  2. 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 <8%). Accuracy, precision and stability tests showed acceptable variation in quality control (QC) samples. This analytical method successfully determined 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. PMID:25255321

  3. A novel strategy for target profiling analysis of bioactive phenylethanoid glycosides in Plantago medicinal plants using ultra-performance liquid chromatography coupled with tandem quadrupole mass spectrometry.

    Science.gov (United States)

    Qi, Meng; Xiong, Aizhen; Geng, Fang; Yang, Li; Wang, Zhengtao

    2012-06-01

    Phenylethanoid glycosides are a group of phenolic compounds with diverse biological activities such as hypotensive, diuretic, and hypoglycemic effects. In this study, a target profiling analysis approach using ultra-performance liquid chromatography coupled with tandem quadrupole mass spectrometry (MS) was established on the basis of parent ion scanning for m/z 161, the characteristic product ion for phenylethanoid glycosides. It was successfully employed to discriminate the chemical composition of phenylethanoid glycosides between Plantaginis Herba and Plantaginis Semen, two medicinal parts of Plantago plants, which are widely used as herbal medicine in China. Totally, 34 phenylethanoid glycosides were characterized and tentatively identified by their retention times, MS, and tandem quadrupole MS (MS/MS) data. Combined with chemometrics analysis of principal component analysis and orthogonal projection to latent structural discriminate analysis, eight of them, especially acteoside and plantamajoside, were picked out and contributed to the chemical distinction between Plantaginis Herba and Plantaginis Semen, which might be responsible for the differences in diuretic and hypotensive effects between the two medicinal parts. This new approach for target profiling provides not only a novel idea for specific analysis of active chemical constituents in the same type, but also a promising and reference method for quality evaluation of traditional Chinese medicines. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. A reflecting time-of-flight mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Tang, X

    1991-01-01

    The design, construction and operation of a reflecting time-of-flight mass spectrometer and the details of the ion mirror are discussed. The principle of velocity focusing with a single-stage ion mirror and the effect of the acceleration region are discussed. The performance of the reflecting instrument is described. Its detection limit is illustrated by observation of [M + H][sup +] ions from [approximately]5-35 femtomoles of various peptides. The factors that affect the resolution are discussed. The principle and operation of the reflecting instrument as a tandem mass spectrometer is described; this involves correlated detection of neutral and ionized fragments. The efficiency, resolution, sensitivity, and mass determination of daughter ions by this method are discussed. Methods of sample preparation are described. By using a nitrocellulose substrate, organic molecular ions as large as bovine insulin (MW 5733) were detected for the first time with low energy (keV) ion bombardment of a solid surface. Many daughter ion spectra resulting from metastable decay of parent ions have been studied. Secondary ions [(CsI)[sub n]Cs][sup +] with n up to [approximately]50 were detected; all clusters were found to be metastable, with most lifetimes <100 [mu]s, and for n>10 the daughter ions are dominant in the mass spectrum. Peptides of mass up to [approximately]2000 u have been studied with the correlated method; the daughter ion spectra were found to be strongly influenced by the identity of the bound cation (H[sup +], Na[sup +], K[sup +], or Ag[sup +]). Many daughter ions formed by known reactions yield structure and sequence information about the peptides. In addition, the [M + Na][sup +] and [M + Ag][sup +] ions decompose by a previously unreported pathway, namely, rearrangement of a C-terminal carboxyl oxygen onto the daughter ion containing the N-terminus. Both the reflected spectra and daughter ion spectra were found useful in peptide sequencing.

  5. Material Classification Using Raw Time-of-Flight Measurements

    KAUST Repository

    Su, Shuochen; Heide, Felix; Swanson, Robin J.; Klein, Jonathan; Callenberg, Clara; Hullin, Matthias; Heidrich, Wolfgang

    2016-01-01

    We propose a material classification method using raw time-of-flight (ToF) measurements. ToF cameras capture the correlation between a reference signal and the temporal response of material to incident illumination. Such measurements encode unique

  6. TANDEM

    Data.gov (United States)

    Federal Laboratory Consortium — The Tandem Van de Graaff facility provides researchers with beams of more than 40 different types of ions - atoms that have been stripped of their electrons. One of...

  7. Energy measurement using a resonator based time-of-flight system

    International Nuclear Information System (INIS)

    Pardo, R.C.; Clifft, B.; Johnson, K.W.; Lewis, R.N.

    1983-01-01

    A resonant pick-up time-of-flight system has been developed for the precise measurement of beam energy at the Argonne Tandem-Linac Accelerator System (ATLAS). The excellent timing characteristics available with ATLAS beams make it desirable to design the beam transport system to be isochronous. The advantages of the resonant time-of-flight system over other energy analysis systems such as the dispersive magnet system are numerous. The system is non-interceptive and non-destructive and preserves the beam phase space. It is non-dispersive. Path length variations are not introduced into the beam which would reduce the timing resolution. It has a large signal-to-noise ratio when compared to non-resonant beam pick-up techniques. It provides the means to precisely set the linac energy and potentially to control the energy in a feedback loop. Finally, the resonant pick-up time-of-flight system is less expensive than an equivalent magnetic system. It consists of two beam-excited resonators, associated electronics to decode the information, a computer interface to the linac PDP 11/34 control computer, and software to analyze the information and deduce the measured beam energy. This report describes the system and its components and gives a schematic overview

  8. Analytical properties of time-of-flight PET data

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Sanghee; Ahn, Sangtae; Quanzheng, Li; Leahy, Richard M [Signal and Image Processing Institute, University of Southern California, Los Angeles, CA 90089 (United States)], E-mail: leahy@sipi.usc.edu

    2008-06-07

    We investigate the analytical properties of time-of-flight (TOF) positron emission tomography (PET) sinograms, where the data are modeled as line integrals weighted by a spatially invariant TOF kernel. First, we investigate the Fourier transform properties of 2D TOF data and extend the 'bow-tie' property of the 2D Radon transform to the time-of-flight case. Second, we describe a new exact Fourier rebinning method, TOF-FOREX, based on the Fourier transform in the time-of-flight variable. We then combine TOF-FOREX rebinning with a direct extension of the projection slice theorem to TOF data, to perform fast 3D TOF PET image reconstruction. Finally, we illustrate these properties using simulated data.

  9. Analytical properties of time-of-flight PET data

    Science.gov (United States)

    Cho, Sanghee; Ahn, Sangtae; Li, Quanzheng; Leahy, Richard M.

    2008-06-01

    We investigate the analytical properties of time-of-flight (TOF) positron emission tomography (PET) sinograms, where the data are modeled as line integrals weighted by a spatially invariant TOF kernel. First, we investigate the Fourier transform properties of 2D TOF data and extend the 'bow-tie' property of the 2D Radon transform to the time-of-flight case. Second, we describe a new exact Fourier rebinning method, TOF-FOREX, based on the Fourier transform in the time-of-flight variable. We then combine TOF-FOREX rebinning with a direct extension of the projection slice theorem to TOF data, to perform fast 3D TOF PET image reconstruction. Finally, we illustrate these properties using simulated data.

  10. Analytical properties of time-of-flight PET data

    International Nuclear Information System (INIS)

    Cho, Sanghee; Ahn, Sangtae; Li Quanzheng; Leahy, Richard M

    2008-01-01

    We investigate the analytical properties of time-of-flight (TOF) positron emission tomography (PET) sinograms, where the data are modeled as line integrals weighted by a spatially invariant TOF kernel. First, we investigate the Fourier transform properties of 2D TOF data and extend the 'bow-tie' property of the 2D Radon transform to the time-of-flight case. Second, we describe a new exact Fourier rebinning method, TOF-FOREX, based on the Fourier transform in the time-of-flight variable. We then combine TOF-FOREX rebinning with a direct extension of the projection slice theorem to TOF data, to perform fast 3D TOF PET image reconstruction. Finally, we illustrate these properties using simulated data

  11. Analytical properties of time-of-flight PET data

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Sanghee; Ahn, Sangtae; Li Quanzheng; Leahy, Richard M [Signal and Image Processing Institute, University of Southern California, Los Angeles, CA 90089 (United States)], E-mail: leahy@sipi.usc.edu

    2008-06-07

    We investigate the analytical properties of time-of-flight (TOF) positron emission tomography (PET) sinograms, where the data are modeled as line integrals weighted by a spatially invariant TOF kernel. First, we investigate the Fourier transform properties of 2D TOF data and extend the 'bow-tie' property of the 2D Radon transform to the time-of-flight case. Second, we describe a new exact Fourier rebinning method, TOF-FOREX, based on the Fourier transform in the time-of-flight variable. We then combine TOF-FOREX rebinning with a direct extension of the projection slice theorem to TOF data, to perform fast 3D TOF PET image reconstruction. Finally, we illustrate these properties using simulated data.

  12. Liquid chromatography, in combination with a quadrupole time-of-flight instrument (LC QTOF), with sequential window acquisition of all theoretical fragment-ion spectra (SWATH) acquisition: systematic studies on its use for screenings in clinical and forensic toxicology and comparison with information-dependent acquisition (IDA).

    Science.gov (United States)

    Roemmelt, Andreas T; Steuer, Andrea E; Poetzsch, Michael; Kraemer, Thomas

    2014-12-02

    Forensic and clinical toxicological screening procedures are employing liquid chromatography-tandem mass spectrometry (LC-MS/MS) techniques with information-dependent acquisition (IDA) approaches more and more often. It is known that the complexity of a sample and the IDA settings might prevent important compounds from being triggered. Therefore, data-independent acquisition (DIA) methods should be more suitable for systematic toxicological analysis (STA). The DIA method sequential window acquisition of all theoretical fragment-ion spectra (SWATH), which uses Q1 windows of 20-35 Da for data-independent fragmentation, was systematically investigated for its suitability for STA. Quality of SWATH-generated mass spectra were evaluated with regard to mass error, relative abundance of the fragments, and library hits. With the Q1 window set to 20-25 Da, several precursors pass Q1 at the same time and are fragmented, thus impairing the library search algorithms to a different extent: forward fit was less affected than reverse fit and purity fit. Mass error was not affected. The relative abundance of the fragments was concentration dependent for some analytes and was influenced by cofragmentation, especially of deuterated analogues. Also, the detection rate of IDA compared to SWATH was investigated in a forced coelution experiment (up to 20 analytes coeluting). Even using several different IDA settings, it was observed that IDA failed to trigger relevant compounds. Screening results of 382 authentic forensic cases revealed that SWATH's detection rate was superior to IDA, which failed to trigger ∼10% of the analytes.

  13. Focusing procedures in time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Ioanoviciu, D.

    2002-01-01

    Time-of-flight mass spectrometry is a fast growing field due to its ability to handle very fast processes and due to its theoretically unlimited mass range. The performances of the time-of-flight mass analysers are heavily dependent on the progress in ion optics, a periodically reviewed field. In this presentation the various focusing procedures in time-of-flight mass spectrometry are reviewed. For ions of the same charge and mass flight time differences result from different potentials at the location of formation and from the initial velocity spread. There is no simultaneous space and velocity focusing in time-of-flight mass spectrometry. Space focusing of first and second order can be reached in time-of-flight mass analysers having two homogeneous electric field ion sources followed by a field free space in front of the detector. Single and double stage homogeneous electric field mirrors can focus in time ions of different energies. These different energies result when ions leaving different initial sites and arriving simultaneously to an intermediate space focus. Convenient mass dispersion can be obtained by including a mirror. Initial velocity focusing is obtained by the delayed extraction procedure in drift space and mirror time-of-flight mass analysers. Post source pulse focusing aims at the same purpose. Ion source electrodes of hyperbolic shape, operated by high voltage pulses can bring major improvements of the resolution, especially at high masses. For each focusing procedure the geometric and/or electric conditions are given as well as the aberrations allowing the mass resolution determination. The various focusing procedures are compared and a prediction of their future performances was tempted. (author)

  14. Identification of AKB-48 and 5F-AKB-48 Metabolites in Authentic Human Urine Samples Using Human Liver Microsomes and Time of Flight Mass Spectrometry.

    Science.gov (United States)

    Vikingsson, Svante; Josefsson, Martin; Gréen, Henrik

    2015-01-01

    The occurrence of structurally related synthetic cannabinoids makes the identification of unique markers of drug intake particularly challenging. The aim of this study was to identify unique and abundant metabolites of AKB-48 and 5F-AKB-48 for toxicological screening in urine. Investigations of authentic urine samples from forensic cases in combination with human liver microsome (HLM) experiments were used for identification of metabolites. HLM incubations of AKB-48 and 5F-AKB-48 along with 35 urine samples from authentic cases were analyzed with liquid chromatography quadrupole tandem time of flight mass spectrometry. Using HLMs 41 metabolites of AKB-48 and 37 metabolites of 5F-AKB-48 were identified, principally represented by hydroxylation but also ketone formation and dealkylation. Monohydroxylated metabolites were replaced by di- and trihydroxylated metabolites within 30 min. The metabolites from the HLM incubations accounted for on average 84% (range, 67-100) and 91% (range, 71-100) of the combined area in the case samples for AKB-48 and 5F-AKB-48, respectively. While defluorinated metabolites accounted for on average 74% of the combined area after a 5F-AKB-48 intake only a few identified metabolites were shared between AKB-48 and 5F-AKB-48, illustrating the need for a systematic approach to identify unique metabolites. HLMs in combination with case samples seem suitable for this purpose. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  15. The statistical chopper in the time-of-flight technique

    International Nuclear Information System (INIS)

    Albuquerque Vieira, J. de.

    1975-12-01

    A detailed study of the 'statistical' chopper and of the method of analysis of the data obtained by this technique is made. The study includes the basic ideas behind correlation methods applied in time-of-flight techniques; comparisons with the conventional chopper made by an analysis of statistical errors; the development of a FORTRAN computer programme to analyse experimental results; the presentation of the related fields of work to demonstrate the potential of this method and suggestions for future study together with the criteria for a time-of-flight experiment using the method being studied [pt

  16. Neutron Time-Of-Flight (n_TOF) experiment

    CERN Multimedia

    Brugger, M; Kaeppeler, F K; Jericha, E; Cortes rossell, G P; Riego perez, A; Baccomi, R; Laurent, B G; Griesmayer, E; Leeb, H; Dressler, M; Cano ott, D; Variale, V; Ventura, A; Carrillo de albornoz trillo, A; Andrzejewski, J J; Pavlik, A F; Kadi, Y; Zanni vlastou, R; Krticka, M; Kokkoris, M; Praena rodriguez, A J; Cortes giraldo, M A; Perkowski, J; Losito, R; Audouin, L; Weiss, C; Tagliente, G; Wallner, A; Woods, P J; Mengoni, A; Guerrero sanchez, C G; Tain enriquez, J L; Vlachoudis, V; Calviani, M; Junghans, A R; Reifarth, R; Mendoza cembranos, E; Quesada molina, J M; Babiano suarez, V; Schumann, M D; Tsinganis, A; Rauscher, T; Calvino tavares, F; Mingrone, F; Gonzalez romero, E M; Colonna, N; Negret, A L; Chiaveri, E; Milazzo, P M; De almeida carrapico, C A; Castelluccio, D M

    The neutron time-of-flight facility n_TOF at CERN, Switzerland, operational since 2001, delivers neutrons using the Proton Synchrotron (PS) 20 GeV/c proton beam impinging on a lead spallation target. The facility combines a very high instantaneous neutron flux, an excellent time of flight resolution due to the distance between the experimental area and the production target (185 meters), a low intrinsic background and a wide range of neutron energies, from thermal to GeV neutrons. These characteristics provide a unique possibility to perform neutron-induced capture and fission cross-section measurements for applications in nuclear astrophysics and in nuclear reactor technology.

  17. Tandem mass spectrometry at low kinetic energy

    International Nuclear Information System (INIS)

    Cooks, R.G.; Hand, O.W.

    1987-01-01

    Recent progress in mass spectrometry, as applied to molecular analysis, is reviewed with emphasis on tandem mass spectrometry. Tandem instruments use multiple analyzers (sector magnets, quadrupole mass filters and time-of-flight devices) to select particular molecules in ionic form, react them in the gas-phase and then record the mass, momenta or kinetic energies of their products. The capabilities of tandem mass spectrometry for identification of individual molecules or particular classes of compounds in complex mixtures are illustrated. Several different types of experiments can be run using a tandem mass spectrometer; all share the feature of sifting the molecular mixture being analyzed on the basis of chemical properties expressed in terms of ionic mass, kinetic energy or charge state. Applications of mass spectrometry to biological problems often depend upon desorption methods of ionization in which samples are bombarded with particle beams. Evaporation of preformed charged species from the condensed phase into the vacuum is a particularly effective method of ionization. It is suggested that the use of accelerator mass spectrometers be extended to include problems of molecular analysis. In such experiments, low energy tandem mass spectrometry conducted in the eV or keV range of energies, would be followed by further characterization of the production ion beam using high selective MeV collision processes

  18. Rocket-borne time-of-flight mass spectrometry

    Science.gov (United States)

    Reiter, R. F.

    1976-01-01

    Theoretical and numerical analyses are made of planar, cylindrical and spherical-electrode two-field time-of-flight mass spectrometers in order to optimize their operating conditions. A method is introduced which can improve the resolving power of these instruments by a factor of 7.5. Potential barrier gating in time-of-flight mass spectrometers is also analyzed. Experimental studies of a miniature cylindrical-electrode and a hemispherical-electrode time-of-flight mass spectrometer are presented. Their sensitivity and ability to operate at D-region pressures with an open source make them ideal instruments for D-region ion composition measurements. A sounding rocket experiment package carrying a cylindrical electrode time-of-flight mass spectrometer was launched. The data indicate that essentially 100% of the positive electric charge on positive ions is carried by ions with mass-to-charge ratios greater than 500 below an altitude of 92 km. These heavy charge carriers were present at altitudes up to about 100 km.

  19. Rocket-borne time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Reiter, R.F.

    1976-08-01

    Theoretical and numerical analyses are made of planar-, cylindrical- and spherical-electrode two-field time-of-flight mass spectrometers in order to optimize their operating conditions. A method is introduced which can improve the resolving power of these instruments by a factor of 7.5. Potential barrier gating in time-of-flight mass spectrometers is also analyzed. Experimental studies of a miniature cylindrical-electrode and a hemispherical-electrode time-of-flight mass spectrometer are presented. Their sensitivity and ability to operate at D-region pressures with an open source make them ideal instruments for D-region ion composition measurements. A sounding rocket experiment package carrying a cylindrical electrode time-of-flight mass spectrometer was launched. The data indicate that essentially 100% of the positive electric charge on positive ions is carried by ions with mass-to-charge ratios greater than 500 below an altitude of 92 km. These heavy charge carriers were present at altitudes up to about 100 km

  20. Magnetic excitations studied with time-of-flight spectroscopy

    International Nuclear Information System (INIS)

    Rainford, B.

    1996-01-01

    An introduction to time-of-flight neutron spectroscopy is presented in the context of the study of magnetic materials. Examples are taken from the class of rare earth and actinide magnetic materials known as 'strongly correlated electron' systems. (author) 11 figs., 24 refs

  1. Time-of-flight positron emission tomography and associated detectors

    International Nuclear Information System (INIS)

    Vacher, J.; Allemand, R.; Campagnolo, R.

    1983-04-01

    An analysis of the timing capabilities of the detectors (scintillators and photomultipliers) in time-of-flight positron emission tomography is presented. The advantages of BaF 2 compared with CsF for the futur tomographs are evaluated [fr

  2. Magnetic excitations studied with time-of-flight spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Rainford, B [Southampton Univ. (United Kingdom). Dept. of Physics

    1996-11-01

    An introduction to time-of-flight neutron spectroscopy is presented in the context of the study of magnetic materials. Examples are taken from the class of rare earth and actinide magnetic materials known as `strongly correlated electron` systems. (author) 11 figs., 24 refs.

  3. Multichannel analyzer for the neutron time-of-flight spectrometer

    International Nuclear Information System (INIS)

    Vojter, A.P.; Slyisenko, V.Yi.; Doronyin, M.Yi.; Maznij, Yi.O.; Vasil'kevich, O.A.; Golyik, V.V.; Koval'ov, O.M.; Kopachov, V.Yi.; Savchuk, V.G.

    2010-01-01

    New multichannel time-of-flight spectrometer for the measurement of the energy and angular distributions of neutrons from the WWWR-M reactor is considered. This spectrometer has been developed for the replacement of the previous one to increase the number of channels and measurement precision, reduce the time of channel tuning and provide the automatic monitoring during the experiment.

  4. Highly segmented, high resolution time-of-flight system

    Energy Technology Data Exchange (ETDEWEB)

    Nayak, T.K.; Nagamiya, S.; Vossnack, O.; Wu, Y.D.; Zajc, W.A. [Columbia Univ., New York, NY (United States); Miake, Y.; Ueno, S.; Kitayama, H.; Nagasaka, Y.; Tomizawa, K.; Arai, I.; Yagi, K [Univ. of Tsukuba, (Japan)

    1991-12-31

    The light attenuation and timing characteristics of time-of-flight counters constructed of 3m long scintillating fiber bundles of different shapes and sizes are presented. Fiber bundles made of 5mm diameter fibers showed good timing characteristics and less light attenuation. The results for a 1.5m long scintillator rod are also presented.

  5. A neutron time-of-flight data acquisition system

    International Nuclear Information System (INIS)

    Morris, D.V.

    1983-10-01

    A neutron time-of-flight scaler system is described for use with the Harwell Linac. The equipment is sufficiently versatile to be used with several types of computers although normally used with DEC PDP 11/45 and PDP 11/34. Using a combination of different input and memory boards most types of experiments can be accommodated. (author)

  6. A novel ion cooling trap for multi-reflection time-of-flight mass spectrograph

    Energy Technology Data Exchange (ETDEWEB)

    Ito, Y., E-mail: yito@riken.jp [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8577 (Japan); Schury, P. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8577 (Japan); New Mexico State University, Department Chemistry and Biochemistry, Las Cruces, NM 88003 (United States); Wada, M.; Naimi, S. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Smorra, C. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Max-Planck-Institut für Kernphysik, Saupfercheckweg 1, D-69117 Heidelberg (Germany); Sonoda, T. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Mita, H. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8577 (Japan); Takamine, A. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Aoyama Gakuin University, 4-4-25 Shibuya, Shibuya-ku, Tokyo 150-8366 (Japan); Okada, K. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Sophia University, 7-1 Kioi-cho, Chiyoda-ku, Tokyo 102-8554 (Japan); Ozawa, A. [University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8577 (Japan); Wollnik, H. [SLOWRI Team, Nishina Accelerator-Based Research Center, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); New Mexico State University, Department Chemistry and Biochemistry, Las Cruces, NM 88003 (United States)

    2013-12-15

    Highlights: • Fast cooling time: 2 ms. • High efficiency: ≈27% for {sup 23}Na{sup +} and ≈5.1% for {sup 7}Li{sup +}. • 100% Duty cycle with double trap system. -- Abstract: A radiofrequency quadrupole ion trap system for use with a multi-reflection time-of-flight mass spectrograph (MRTOF) for short-lived nuclei has been developed. The trap system consists of two different parts, an asymmetric taper trap and a flat trap. The ions are cooled to a sufficient small bunch for precise mass measurement with MRTOF in only 2 ms cooling time in the flat trap, then orthogonally ejected to the MRTOF for mass analysis. A trapping efficiency of ≈27% for {sup 23}Na{sup +} and ≈5.1% for {sup 7}Li{sup +} has been achieved.

  7. Detection and quantification of neurotensin in human brain tissue by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

    DEFF Research Database (Denmark)

    Gobom, J; Kraeuter, K O; Persson, R

    2000-01-01

    A method was developed for mass spectrometric detection of neurotensin (NT)-like immunoreactivity and quantification of NT in human brain tissue. The method is based on immunoprecipitation followed by analysis using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF......-MS). The identity of the major component of the immunoprecipitates as neurotensin was confirmed by fragment ion analysis on an electrospray ionization quadrupole time-of-flight instrument. MALDI-TOF-MS quantification of NT was achieved using stable-isotope-labeled NT as the internal standard, yielding an error...

  8. UTOFIA: an underwater time-of-flight image acquisition system

    Science.gov (United States)

    Driewer, Adrian; Abrosimov, Igor; Alexander, Jonathan; Benger, Marc; O'Farrell, Marion; Haugholt, Karl Henrik; Softley, Chris; Thielemann, Jens T.; Thorstensen, Jostein; Yates, Chris

    2017-10-01

    In this article the development of a newly designed Time-of-Flight (ToF) image sensor for underwater applications is described. The sensor is developed as part of the project UTOFIA (underwater time-of-flight image acquisition) funded by the EU within the Horizon 2020 framework. This project aims to develop a camera based on range gating that extends the visible range compared to conventional cameras by a factor of 2 to 3 and delivers real-time range information by means of a 3D video stream. The principle of underwater range gating as well as the concept of the image sensor are presented. Based on measurements on a test image sensor a pixel structure that suits best to the requirements has been selected. Within an extensive characterization underwater the capability of distance measurements in turbid environments is demonstrated.

  9. Pulse Based Time-of-Flight Range Sensing.

    Science.gov (United States)

    Sarbolandi, Hamed; Plack, Markus; Kolb, Andreas

    2018-05-23

    Pulse-based Time-of-Flight (PB-ToF) cameras are an attractive alternative range imaging approach, compared to the widely commercialized Amplitude Modulated Continuous-Wave Time-of-Flight (AMCW-ToF) approach. This paper presents an in-depth evaluation of a PB-ToF camera prototype based on the Hamamatsu area sensor S11963-01CR. We evaluate different ToF-related effects, i.e., temperature drift, systematic error, depth inhomogeneity, multi-path effects, and motion artefacts. Furthermore, we evaluate the systematic error of the system in more detail, and introduce novel concepts to improve the quality of range measurements by modifying the mode of operation of the PB-ToF camera. Finally, we describe the means of measuring the gate response of the PB-ToF sensor and using this information for PB-ToF sensor simulation.

  10. Time-of-flight detector with KBr working medium

    International Nuclear Information System (INIS)

    Arvanov, A.N.; Gavalyan, V.G.; Lorikyan, M.P.

    1983-01-01

    A detector of controlled secondary electron emission as a 3-electrode focusing electrostatic system of the photomultiplier input chamber having a microchannel electron plate herringbone assembly with the total gain of approXimately 10 7 is described. A controlled secondary emission emitter based on MgO or KBr is installed as a cathode. The detector is designed for time-of-flight spectrometers. The time resolution is < or approximately equal to 0.5 ns. The time-of-flight system realized on the base of such two detectors has 100% detection efficiency and it is ''transparent'' for an identified particle. Its characteristics for α particle, deuteron and proton detection are estimated

  11. Time of flight measurement on the SOFIA experiment

    International Nuclear Information System (INIS)

    Bail, A.; Taieb, J.; Chatillon, A.; Belier, G.; Laurent, B.; Pellereau, E.

    2011-01-01

    The SOFIA experiment, which will be held at GSI (Darmstadt (Germany)) will allow to completely determine the mass and charge numbers of fragments produced in the fission reaction of radioactive actinides in reverse kinematics. Therefore, a dedicated setup has been developed for the Time of Flight measurement of relativistic heavy ions. The studies, which led to the choice of the adequate plastic scintillators and photomultipliers, are presented. Tests have been undertaken with the ELSA laser and electron beam facility. They shown that a suitable choice would be EJ-232 plastic scintillator for the ToF wall and EJ-232Q for the start detector and Hamamatsu H6533 and H10580 photomultipliers. This was confirmed by two test experiments realized at GSI with relativistic heavy ion beam ( 56 Fe and 238 U), where a time of flight resolution better than 20 ps FWHM was reached. (authors)

  12. Time of flight measurement on the SOFIA experiment

    Energy Technology Data Exchange (ETDEWEB)

    Bail, A.; Taieb, J.; Chatillon, A.; Belier, G.; Laurent, B.; Pellereau, E. [CEA/DAM/DIF, Arpajon (France)

    2011-07-01

    The SOFIA experiment, which will be held at GSI (Darmstadt (Germany)) will allow to completely determine the mass and charge numbers of fragments produced in the fission reaction of radioactive actinides in reverse kinematics. Therefore, a dedicated setup has been developed for the Time of Flight measurement of relativistic heavy ions. The studies, which led to the choice of the adequate plastic scintillators and photomultipliers, are presented. Tests have been undertaken with the ELSA laser and electron beam facility. They shown that a suitable choice would be EJ-232 plastic scintillator for the ToF wall and EJ-232Q for the start detector and Hamamatsu H6533 and H10580 photomultipliers. This was confirmed by two test experiments realized at GSI with relativistic heavy ion beam ({sup 56}Fe and {sup 238}U), where a time of flight resolution better than 20 ps FWHM was reached. (authors)

  13. Screening and identification of steroidal saponins from Anemarrhena asphodeloides employing UPLC tandem triple quadrupole linear ion trap mass spectrometry.

    Science.gov (United States)

    Xia, Yong-Gang; Guo, Xin-Dong; Liang, Jun; Yang, Bing-You; Kuang, Hai-Xue

    2017-09-01

    This study presents a practical and valid strategy for the screening and structural characterization of Anemarrhena asphodeloides Bge steroidal saponins (SSs) using ultra-high performance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometry. The whole analytical protocols integrate four-step procedures in the positive mode: (1) rational deduction of mass fragmentation pathways of A. asphodeloides SSs; (2) untargeted screening of potential A. asphodeloides SSs by multiple-ion monitoring-information-dependent-acquiring-enhanced product ion (MIM-IDA-EPI) scan through reverse phase liquid chromatography; (3) comprehensive construction of an ammoniated precursor ion database by combining untargeted MIM-IDA-EPI scans and data literature; and (4) structural interpretation of targeted A. asphodeloides SSs using MIM-IDA-EPI and multiple reaction monitoring (MRM)-IDA-EPI with an energy-resolved technique. The protocols were used to analyze SSs in A. asphodeloides; of the 87 detected SSs that were unambiguously characterized or tentatively identified, 19 compounds were the first to be reported from A. asphodeloides and 13 ones were characterized as potential new compounds. Accuracy of the analytical procedure was demonstrated by structural identification of three SSs by NMR spectroscopy. The proposed schemes hold an excellent promise in the structural prediction and interpretation of complex SSs from plant medicines by mass spectrometry. Copyright © 2017 Elsevier Inc. All rights reserved.

  14. Trajectory bending and energy spreading of charged ions in time-of-flight telescopes used for ion beam analysis

    International Nuclear Information System (INIS)

    Laitinen, Mikko; Sajavaara, Timo

    2014-01-01

    Carbon foil time pick-up detectors are widely used in pairs in ion beam applications as time-of-flight detectors. These detectors are suitable for a wide energy range and for all ions but at the lowest energies the tandem effect limits the achievable time of flight and therefore the energy resolution. Tandem effect occurs when an ion passes the first carbon foil of the timing detector and its charge state is changed. As the carbon foil of the first timing detector has often a non-zero voltage the ion can accelerate or decelerate before and after the timing detector. The combination of different charge state properties before and after the carbon foil now induces spread to the measured times of flight. We have simulated different time pick-up detector orientations, voltages, ions and ion energies to examine the tandem effect in detail and found out that the individual timing detector orientation and the average ion charge state have a very small influence to the magnitude of the tandem effect. On the other hand, the width of the charge state distribution for particular ion and energy in the first carbon foil, and the carbon foil voltage contributes linearly to the magnitude of the tandem effect. In the simulations low energy light ion trajectories were observed to bend in the electric fields of the first timing gate, and the magnitude of this bending was studied. It was found out that 50–150 keV proton trajectories can even bend outside the second timing gate

  15. Time coder for slow neutron time-of-flight spectrometer

    International Nuclear Information System (INIS)

    Grashilin, V.A.; Ofengenden, R.G.

    1988-01-01

    Time coder for slow neutron time-of-flight spectrometer is described. The time coder is of modular structure, is performed in the CAMAC standard and operates on line with DVK-2 computer. The main coder units include supporting generator, timers, time-to-digital converter, memory unit and crate controller. Method for measuring background symmetrically to the effect is proposed for a more correct background accounting. 4 refs.; 1 fig

  16. Time of flight spectrometry in heavy ions backscattering analysis

    International Nuclear Information System (INIS)

    Chevarier, A.; Chevarier, N.

    1983-05-01

    Time of flight spectrometry for backscattering analysis of MeV heavy ions is proposed. The capabilities and limitations of this method are investigated. Depth and mass resolution obtained in measurements of oxide films thickness as well as in GaAs layers analysis are presented. The importance of minimizing pile-up without significant loss of resolution by use of an adequate absorber set just in front of the rear detector is underlined

  17. Detailed investigation of a time-of-flight neutron spectrometer

    International Nuclear Information System (INIS)

    Elevant, T.; Trostell, B.

    1981-02-01

    Properties of a neutron spectrometer and telescope, based on double neutron interaction in hydrogen based scintillators and neutron time-of-flight technique, have been investigated in detail. Theoretical scaling of the resolutions with the flight path length and scattering angle have been confirmed by experimental results. Important parameters in connection with calibration of the spectrometer are discussed and calculated relative resolutions of the ion temperature are shown when applied to a fusion deuterium plasma. (Auth.)

  18. The time-of-flight detector of the DIRAC experiment

    International Nuclear Information System (INIS)

    Adeva, B.; Gallas, M.V.; Gomez, F.; Lopez-Agueera, A.; Nunez-Pardo, T.; Plo, M.; Rodriguez, A.M.; Rodriguez, X.M.; Saborido, J.J.; Santamarina, C.; Tobar, M.J.; Vazquez, P.

    2002-01-01

    The construction and performance of a large area time-of-flight detector for the DIRAC experiment at CERN is reported. With an average time resolution of 123 ps per counter at rates up to 1 MHz, it allows excellent separation of pπ - from π + π - pairs up to 4.6 GeV/c momentum, as well as of Coulomb-correlated pion pairs from accidentals. The optimization of scintillator material, photomultiplier performance and readout electronics is described

  19. A time of flight detector for high energy heavy particles

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Z; O` Connor, D J [Newcastle Univ., NSW (Australia). Dept. of Physics

    1994-12-31

    As a commonly used method to measure the energy of a particle with known mass, the flight time of the particle travelling over a certain distance is measured. A detector based on this principle is called a time-of-flight (TOF) detector which has attracted interests constantly during the last 15 years. For high energy heavy particle energy detection, TOF detector is an appropriated choice and such a system, developed recently, is described in this paper. 8 refs., 3 figs.

  20. A time of flight detector for high energy heavy particles

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Z.; O`Connor, D.J. [Newcastle Univ., NSW (Australia). Dept. of Physics

    1993-12-31

    As a commonly used method to measure the energy of a particle with known mass, the flight time of the particle travelling over a certain distance is measured. A detector based on this principle is called a time-of-flight (TOF) detector which has attracted interests constantly during the last 15 years. For high energy heavy particle energy detection, TOF detector is an appropriated choice and such a system, developed recently, is described in this paper. 8 refs., 3 figs.

  1. KELVIN rare gas time-of-flight program

    International Nuclear Information System (INIS)

    Vernon, M.

    1981-03-01

    The purpose of this appendix is to explain in detail the procedure for performing time-of-flight (TOF) calibration measurements. The result of the calibration measurements is to assign a correct length (L) to the path the molecules travel in a particular experimental configuration. In conjunction with time information (t) a velocity distribution (L/t) can then be determined. The program KELVIN is listed

  2. Simultaneous determination of 9 heterocyclic aromatic amines in pork products by liquid chromatography coupled with triple quadrupole tandem mass spectrometry

    Science.gov (United States)

    Shen, X. C.; Zhang, Y. L.; Cui, Y. Q.; Xu, L. Y.; Li, X.; Qi, J. H.

    2017-07-01

    Heterocyclic aromatic amines (HAAs) are potent mutagens that formed at high temperature in cooked, protein-rich food. Owing to their frequent intake, an accurate method is essential to access human health risk of HAAs exposure through detecting these compounds in various heat-treated meat products. In this study, a liquid chromatography-electrospray tandem mass spectrometry (LC--ESI-MS/MS) method was developed to perform the determination of 9 mutagenic heterocyclic amines (HAAs) in meat samples with multiple reaction monitoring (MRM) mode. Ultrasound assisted extraction and diatomaceous earth was employed to extract HAAs from food samples, and the analytes were purified and enriched using tandem solid phase extraction, with propyl sulfonic acid coupled to a C18 cartridge. Two parameters, extraction time and eluent, were carefully optimized to improve the extraction and purification efficiency. The LC separation was carried out using a Zorbax SB-C18 (3.5 μm particle size, 2.1 × 150 mm i.d.) column and optimized some parameters, such as pH, concentration and volume. Under the optimal experimental conditions, recoveries ranged from 52.97% to 97.11% with good quality parameters: limit of detection values between 0.02 and 0.24 ng mL-1, linearity (R2>0.998), and run-to-run and day-to-day precisions lower than 9.81% achieved. To evaluate the performance of the method in high throughput analysis of complex meat samples, the LC-MS/MS method was applied to the analysis of HAAs in three food samples, and the results demonstrated that the method can be used for the trace determination of HAAs in pork samples.

  3. Hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry for highly rapid and sensitive analysis of underivatized amino acids in functional foods.

    Science.gov (United States)

    Zhou, Guisheng; Pang, Hanqing; Tang, Yuping; Yao, Xin; Mo, Xuan; Zhu, Shaoqing; Guo, Sheng; Qian, Dawei; Qian, Yefei; Su, Shulan; Zhang, Li; Jin, Chun; Qin, Yong; Duan, Jin-ao

    2013-05-01

    This work presented a new analytical methodology based on hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry in multiple-reaction monitoring mode for analysis of 24 underivatized free amino acids (FAAs) in functional foods. The proposed method was first reported and validated by assessing the matrix effects, linearity, limit of detections and limit of quantifications, precision, repeatability, stability and recovery of all target compounds, and it was used to determine the nutritional substances of FAAs in ginkgo seeds and further elucidate the nutritional value of this functional food. The result showed that ginkgo seed turned out to be a good source of FAAs with high levels of several essential FAAs and to have a good nutritional value. Furthermore, the principal component analysis was performed to classify the ginkgo seed samples on the basis of 24 FAAs. As a result, the samples could be mainly clustered into three groups, which were similar to areas classification. Overall, the presented method would be useful for the investigation of amino acids in edible plants and agricultural products.

  4. Determination of short chain chlorinated paraffins in water by stir bar sorptive extraction-thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Tölgyessy, P; Nagyová, S; Sládkovičová, M

    2017-04-21

    A simple, robust, sensitive and environment friendly method for the determination of short chain chlorinated paraffins (SCCPs) in water using stir bar sorptive extraction (SBSE) coupled to thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry (TD-GC-QqQ-MS/MS) was developed. SBSE was performed using 100mL of water sample, 20mL of methanol as a modifier, and a commercial sorptive stir bar (with 10mm×0.5mm PDMS layer) during extraction period of 16h. After extraction, the sorptive stir bar was thermally desorbed and online analysed by GC-MS/MS. Method performance was evaluated for MilliQ and surface water spiked samples. For both types of matrices, a linear dynamic range of 0.5-3.0μgL -1 with correlation coefficients >0.999 and relative standard deviations (RSDs) of the relative response factors (RRFs) <12% was established. The limits of quantification (LOQs) of 0.06 and 0.08μgL -1 , and the precision (repeatability) of 6.4 and 7.7% (RSDs) were achieved for MilliQ and surface water, respectively. The method also showed good robustness, recovery and accuracy. The obtained performance characteristics indicate that the method is suitable for screening and monitoring and compliance checking with environmental quality standards (EQS, set by the EU) for SCCPs in surface waters. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Application of dispersive solid-phase extraction and ultra-fast liquid chromatography-tandem quadrupole mass spectrometry in food additive residue analysis of red wine.

    Science.gov (United States)

    Chen, Xiao-Hong; Zhao, Yong-Gang; Shen, Hao-Yu; Jin, Mi-Cong

    2012-11-09

    A novel and effective dispersive solid-phase extraction (dSPE) procedure with rapid magnetic separation using ethylenediamine-functionalized magnetic polymer as an adsorbent was developed. The new procedure had excellent clean-up ability for the selective removal of the matrix in red wine. An accurate, simple, and rapid analytical method using ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the simultaneous determination of nine food additives (i.e., acesulfame, saccharin, sodium cyclamate, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid, and neotame) in red wine was also used and validated. Recoveries ranging from 78.5% to 99.2% with relative standard deviations ranging from 0.46% to 6.3% were obtained using the new method. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9993. The limits of quantification for the nine food additives were between 0.10 μg/L and 50.0 μg/L. The proposed dSPE-UFLC-MS/MS method was successfully applied in the food-safety risk monitoring of real red wine in Zhejiang Province, China. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

  6. 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.

  7. Development and Validation of a Multiresidue Method for the Determination of Pesticides in Dry Samples (Rice and Wheat Flour) Using Liquid Chromatography/Triple Quadrupole Tandem Mass Spectrometry.

    Science.gov (United States)

    Grande-Martínez, Ángel; Arrebola, Francisco Javier; Moreno, Laura Díaz; Vidal, José Luis Martínez; Frenich, Antonia Garrido

    2015-01-01

    A rapid and sensitive multiresidue method was developed and validated for the determination of around 100 pesticides in dry samples (rice and wheat flour) by ultra-performance LC coupled to a triple quadrupole mass analyzer working in tandem mode (UPLC/QqQ-MS/MS). The sample preparation step was optimized for both matrixes. Pesticides were extracted from rice samples using aqueous ethyl acetate, while aqueous acetonitrile extraction [modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method] was used for wheat flour matrixes. In both cases the extracts were then cleaned up by dispersive solid phase extraction with MgSO4 and primary secondary amine+C18 sorbents. A further cleanup step with Florisil was necessary to remove fat in wheat flour. The method was validated at two concentration levels (3.6 and 40 μg/kg for most compounds), obtaining recoveries ranging from 70 to 120%, intraday and interday precision values≤20% expressed as RSDs, and expanded uncertainty values≤50%. The LOQ values ranged between 3.6 and 20 μg/kg, although it was set at 3.6 μg/kg for the majority of the pesticides. The method was applied to the analysis of 20 real samples, and no pesticides were detected.

  8. Time of flight imaging through scattering environments (Conference Presentation)

    Science.gov (United States)

    Le, Toan H.; Breitbach, Eric C.; Jackson, Jonathan A.; Velten, Andreas

    2017-02-01

    Light scattering is a primary obstacle to imaging in many environments. On small scales in biomedical microscopy and diffuse tomography scenarios scattering is caused by tissue. On larger scales scattering from dust and fog provide challenges to vision systems for self driving cars and naval remote imaging systems. We are developing scale models for scattering environments and investigation methods for improved imaging particularly using time of flight transient information. With the emergence of Single Photon Avalanche Diode detectors and fast semiconductor lasers, illumination and capture on picosecond timescales are becoming possible in inexpensive, compact, and robust devices. This opens up opportunities for new computational imaging techniques that make use of photon time of flight. Time of flight or range information is used in remote imaging scenarios in gated viewing and in biomedical imaging in time resolved diffuse tomography. In addition spatial filtering is popular in biomedical scenarios with structured illumination and confocal microscopy. We are presenting a combination analytical, computational, and experimental models that allow us develop and test imaging methods across scattering scenarios and scales. This framework will be used for proof of concept experiments to evaluate new computational imaging methods.

  9. Multivariate Sensitivity Analysis of Time-of-Flight Sensor Fusion

    Science.gov (United States)

    Schwarz, Sebastian; Sjöström, Mårten; Olsson, Roger

    2014-09-01

    Obtaining three-dimensional scenery data is an essential task in computer vision, with diverse applications in various areas such as manufacturing and quality control, security and surveillance, or user interaction and entertainment. Dedicated Time-of-Flight sensors can provide detailed scenery depth in real-time and overcome short-comings of traditional stereo analysis. Nonetheless, they do not provide texture information and have limited spatial resolution. Therefore such sensors are typically combined with high resolution video sensors. Time-of-Flight Sensor Fusion is a highly active field of research. Over the recent years, there have been multiple proposals addressing important topics such as texture-guided depth upsampling and depth data denoising. In this article we take a step back and look at the underlying principles of ToF sensor fusion. We derive the ToF sensor fusion error model and evaluate its sensitivity to inaccuracies in camera calibration and depth measurements. In accordance with our findings, we propose certain courses of action to ensure high quality fusion results. With this multivariate sensitivity analysis of the ToF sensor fusion model, we provide an important guideline for designing, calibrating and running a sophisticated Time-of-Flight sensor fusion capture systems.

  10. TORCH—a Cherenkov based time-of-flight detector

    Energy Technology Data Exchange (ETDEWEB)

    Dijk, M.W.U. van, E-mail: m.vandijk@bristol.ac.uk [H.H. Wills Physics Laboratory, University of Bristol, Tyndall Avenue, Bristol BS8 1TL (United Kingdom); Brook, N.H. [H.H. Wills Physics Laboratory, University of Bristol, Tyndall Avenue, Bristol BS8 1TL (United Kingdom); Castillo García, L. [European Organisation for Nuclear Research (CERN), CH-1211 Geneva 23 (Switzerland); Laboratory for High Energy Physics, Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne (Switzerland); Cowie, E.N.; Cussans, D. [H.H. Wills Physics Laboratory, University of Bristol, Tyndall Avenue, Bristol BS8 1TL (United Kingdom); D' Ambrosio, C. [European Organisation for Nuclear Research (CERN), CH-1211 Geneva 23 (Switzerland); Fopma, J. [Denys Wilkinson Laboratory, University of Oxford, Keble Road, Oxford OX1 3RH (United Kingdom); Forty, R.; Frei, C. [European Organisation for Nuclear Research (CERN), CH-1211 Geneva 23 (Switzerland); Gao, R. [Denys Wilkinson Laboratory, University of Oxford, Keble Road, Oxford OX1 3RH (United Kingdom); Gys, T. [European Organisation for Nuclear Research (CERN), CH-1211 Geneva 23 (Switzerland); Harnew, N.; Keri, T. [Denys Wilkinson Laboratory, University of Oxford, Keble Road, Oxford OX1 3RH (United Kingdom); Piedigrossi, D. [European Organisation for Nuclear Research (CERN), CH-1211 Geneva 23 (Switzerland)

    2014-12-01

    TORCH is an innovative high-precision time-of-flight system to provide particle identification in the difficult intermediate momentum region up to 10 GeV/c. It is also suitable for large-area applications. The detector provides a time-of-flight measurement from the imaging of Cherenkov photons emitted in a 1 cm thick quartz radiator. The photons propagate by total internal reflection to the edge of the quartz plate and are then focused onto an array of photon detectors at the periphery. A time-of-flight resolution of about 10–15 ps per incident charged particle needs to be achieved to allow a three sigma kaon-pion separation up to 10 GeV/c momentum for the TORCH located 9.5 m from the interaction point. Given ∼30 detected photons per incident charged particle, this requires measuring the time-of-arrival of individual photons to about 70 ps. This paper will describe the design of a TORCH prototype involving a number of ground-breaking and challenging techniques.

  11. Isobar Separation in a Multiple-Reflection Time-of-Flight Mass Spectrometer by Mass-Selective Re-Trapping

    Science.gov (United States)

    Dickel, Timo; Plaß, Wolfgang R.; Lippert, Wayne; Lang, Johannes; Yavor, Mikhail I.; Geissel, Hans; Scheidenberger, Christoph

    2017-06-01

    A novel method for (ultra-)high-resolution spatial mass separation in time-of-flight mass spectrometers is presented. Ions are injected into a time-of-flight analyzer from a radio frequency (rf) trap, dispersed in time-of-flight according to their mass-to-charge ratios and then re-trapped dynamically in the same rf trap. This re-trapping technique is highly mass-selective and after sufficiently long flight times can provide even isobaric separation. A theoretical treatment of the method is presented and the conditions for optimum performance of the method are derived. The method has been implemented in a multiple-reflection time-of-flight mass spectrometer and mass separation powers (FWHM) in excess of 70,000, and re-trapping efficiencies of up to 35% have been obtained for the protonated molecular ion of caffeine. The isobars glutamine and lysine (relative mass difference of 1/4000) have been separated after a flight time of 0.2 ms only. Higher mass separation powers can be achieved using longer flight times. The method will have important applications, including isobar separation in nuclear physics and (ultra-)high-resolution precursor ion selection in multiple-stage tandem mass spectrometry. [Figure not available: see fulltext.

  12. Molecular beam studies with a time-of-flight machine

    International Nuclear Information System (INIS)

    Beijerinck, H.C.W.

    1975-01-01

    The study concerns the development of the time-of-flight method for the velocity analysis of molecular beams and its application to the measurement of the velocity dependence of the total cross-section of the noble gases. It reviews the elastic scattering theory, both in the framework of classical mechanics and in the quantum mechanical description. Attention is paid to the semiclassical correspondence of classical particle trajectories with the partial waves of the quantum mechanical solution. The total cross-section and the small angle differential cross-section are discussed with special emphasis on their relation. The results of this chapter are used later to derive the correction on the measured total cross-section due to the finite angular resolution of the apparatus. Reviewed also is the available information on the intermolecular potential of the Ar-Ar system. Then a discussion of the measurement of total cross-sections with the molecular beam method and the time-of-flight method is compared to other methods used. It is shown that the single burst time-of-flight method can be developed into a reliable and well-calibrated method for the analysis of the velocity distribution of molecular beams. A comparison of the single burst time-of-flight method with the cross-correlation time-of-flight method shows that the two methods are complementary and that the specific experimental circumstances determine which method is to be preferred. Molecular beam sources are discussed. The peaking factor formalism is introduced and helps to compare the performance of different types of sources. The effusive and the supersonic source are treated and recent experimental results are given. The multichannel source is treated in more detail. For the opaque mode, an experimental investigation of the velocity distribution and the angular distribution of the flow pattern is presented. Comparison of these results with Monte Carlo calculations for free molecular flow in a cylindrical

  13. Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, Fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques

    NARCIS (Netherlands)

    Nielen, M.W.F.; Engelen, M.C. van; Zuiderent, R.; Ramaker, R.

    2007-01-01

    An emerging trend is recognised in hormone and veterinary drug residue analysis from liquid chromatography tandem mass spectrometry (LC/MS/MS) based screening and confirmation towards accurate mass alternatives such as LC coupled with time-of-flight (TOF), Fourier transform ion cyclotron resonance

  14. 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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    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.

  16. A homemade high-resolution orthogonal-injection time-of-flight mass spectrometer with a heated capillary inlet

    International Nuclear Information System (INIS)

    Guo Changjuan; Huang Zhengxu; Gao Wei; Nian Huiqing; Chen Huayong; Dong Junguo; Shen Guoying; Fu Jiamo; Zhou Zhen

    2008-01-01

    We describe a homemade high-resolution orthogonal-injection time-of-flight (O-TOF) mass spectrometer combing a heated capillary inlet. The O-TOF uses a heated capillary tube combined with a radio-frequency only quadrupole (rf-only quadrupole) as an interface to help the ion transmission from the atmospheric pressure to the low-pressure regions. The principle, configuration of the O-TOF, and the performance of the instrument are introduced in this paper. With electrospray ion source, the performances of the mass resolution, the sensitivity, the mass range, and the mass accuracy are described. We also include our results obtained by coupling atmospheric pressure matrix-assisted laser deporption ionization with this instrument

  17. The development of a time of flight diffractometer, FIONA

    International Nuclear Information System (INIS)

    Goodyear, A.G.; Miller, R.J.R.

    1975-11-01

    A neutron diffractometer, FIONA, has been built at AWRE in order to study structure and equation of state data of materials at high pressures and elevated temperatures. It is required that the sample should be subjected to pressures up to 60 kbar and temperatures up to 800 0 K. There is a further requirement that the diffractometer should have a multi-detector system to make the maximum use of the neutrons available from the 5 MW HERALD reactor. Both these requirements can be met by using a time of flight diffractometer. The instrument is described. (author)

  18. Cluster Tracking with Time-of-Flight Cameras

    DEFF Research Database (Denmark)

    Hansen, Dan Witzner; Hansen, Mads; Kirschmeyer, Martin

    2008-01-01

    We describe a method for tracking people using a time-of-flight camera and apply the method for persistent authentication in a smart-environment. A background model is built by fusing information from intensity and depth images. While a geometric constraint is employed to improve pixel cluster...... coherence and reducing the influence of noise, the EM algorithm (expectation maximization) is used for tracking moving clusters of pixels significantly different from the background model. Each cluster is defined through a statistical model of points on the ground plane. We show the benefits of the time...

  19. The Time-of-Flight Detector for the ALICE experiment

    CERN Document Server

    Williams, M C S

    2002-01-01

    The Multigap Resistive Plate Chamber (MRPC) will be used to build a large Time-of-Flight detector for the ALICEexperiment. It will cover an area of 150 m2 consisting of 160,000 channels of 3.5 x 2.5 cm2 read-out pads. We present the results of the last 2 years of R&D during which we investigated problems associated with scaling up from single cells of 3 x 3 cm2 to strips with active area of 7 × 120 cm2 read out with 96 pads.

  20. Timing properties of a time-of-flight detector

    International Nuclear Information System (INIS)

    Nakagawa, Takahide; Yuasa-Nakagawa, Keiko.

    1989-01-01

    The time resolution of a time-of-flight (T.O.F.) detector which consists of a channel plate detector (CPD) with a central hole and a surface barrier detector (SBD) was measured. A time resolution of 80 psec fwhm was obtained for 8.78 MeV alpha particles. The influence on fast timing of the SBD of alpha particles was carefully studied. The plasma delay time and time resolution of the SBD were found to strongly depend on the electric field strength and properties of the SBD. (author)

  1. Time-of-flight range imaging for underwater applications

    Science.gov (United States)

    Merbold, Hannes; Catregn, Gion-Pol; Leutenegger, Tobias

    2018-02-01

    Precise and low-cost range imaging in underwater settings with object distances on the meter level is demonstrated. This is addressed through silicon-based time-of-flight (TOF) cameras operated with light emitting diodes (LEDs) at visible, rather than near-IR wavelengths. We find that the attainable performance depends on a variety of parameters, such as the wavelength dependent absorption of water, the emitted optical power and response times of the LEDs, or the spectral sensitivity of the TOF chip. An in-depth analysis of the interplay between the different parameters is given and the performance of underwater TOF imaging using different visible illumination wavelengths is analyzed.

  2. Time-of-flight cameras principles, methods and applications

    CERN Document Server

    Hansard, Miles; Choi, Ouk; Horaud, Radu

    2012-01-01

    Time-of-flight (TOF) cameras provide a depth value at each pixel, from which the 3D structure of the scene can be estimated. This new type of active sensor makes it possible to go beyond traditional 2D image processing, directly to depth-based and 3D scene processing. Many computer vision and graphics applications can benefit from TOF data, including 3D reconstruction, activity and gesture recognition, motion capture and face detection. It is already possible to use multiple TOF cameras, in order to increase the scene coverage, and to combine the depth data with images from several colour came

  3. Material Classification Using Raw Time-of-Flight Measurements

    KAUST Repository

    Su, Shuochen

    2016-12-13

    We propose a material classification method using raw time-of-flight (ToF) measurements. ToF cameras capture the correlation between a reference signal and the temporal response of material to incident illumination. Such measurements encode unique signatures of the material, i.e. the degree of subsurface scattering inside a volume. Subsequently, it offers an orthogonal domain of feature representation compared to conventional spatial and angular reflectance-based approaches. We demonstrate the effectiveness, robustness, and efficiency of our method through experiments and comparisons of real-world materials.

  4. Time-of-Flight Positron Emission Tomography with Radiofrequency Phototube

    International Nuclear Information System (INIS)

    Margaryan, A.; Kakoyan, V.; Knyazyan, S.

    2011-01-01

    In this paper γ-detector, based on the radiofrequency (RF) phototube and recently developed fast and ultrafast scintillators, is considered for Time-of-Flight positron emission tomography applications. Timing characteristics of such a device has been investigated by means of a dedicated Monte Carlo code based on the single photon counting concept. Biexponential timing model for scintillators have been used. The calculations have shown that such a timing model is in a good agreement with recently measured data. The timing resolution of -detectors can be significantly improved by using the RF phototube. (authors)

  5. The ALICE Time of Flight Readout System AFRO

    CERN Document Server

    Kluge, A

    1999-01-01

    The ALICE Time of Flight Detector system comprises more than 100.000 channels and covers an area of more than 100 m2. The timing resolution should be better than 150 ps. This combination of requirements poses a major challenge to the readout system. All detector timing measurements are referenced to a unique start signal t0. This signal is generated at the time an event occurs. Timing measurements are performed using a multichannel TDC chip which requires a 40 MHz reference clock signal. The general concept of the readout system is based on a modular architecture. Detector cells are combined to modules of 1024 channels. Each of these modules can be read out and calibrated independently from each other. By distributing a reference signal, a timing relationship between the modules is established. This reference signal can either be the start signal t0 or the TDC-reference clock. The readout architecture is divided into three steps; the TDC controller, the module controller, and the time of flight controller. Th...

  6. Time of flight Laue fiber diffraction studies of perdeuterated DNA

    Energy Technology Data Exchange (ETDEWEB)

    Forsyth, V.T.; Whalley, M.A.; Mahendrasingam, A.; Fuller, W. [Keele Univ. (United Kingdom)] [and others

    1994-12-31

    The diffractometer SXD at the Rutherford Appleton Laboratory ISIS pulsed neutron source has been used to record high resolution time-of-flight Laue fiber diffraction data from DNA. These experiments, which are the first of their kind, were undertaken using fibers of DNA in the A conformation and prepared using deuterated DNA in order to minimis incoherent background scattering. These studies complement previous experiments on instrument D19 at the Institute Laue Langevin using monochromatic neutrons. Sample preparation involved drawing large numbers of these deuterated DNA fibers and mounting them in a parallel array. The strategy of data collection is discussed in terms of camera design, sample environment and data collection. The methods used to correct the recorded time-of-flight data and map it into the final reciprocal space fiber diffraction dataset are also discussed. Difference Fourier maps showing the distribution of water around A-DNA calculated on the basis of these data are compared with results obtained using data recorded from hydrogenated A-DNA on D19. Since the methods used for sample preparation, data collection and data processing are fundamentally different for the monochromatic and Laue techniques, the results of these experiments also afford a valuable opportunity to independently test the data reduction and analysis techniques used in the two methods.

  7. Time-of-flight neutron diffractometer for monocrystal study

    International Nuclear Information System (INIS)

    Anan'ev, B.N.; Balagurov, A.M.; Barabash, I.P.; Georgiu, Z.; Shibaev, V.D.

    1979-01-01

    The design of a neutron diffractometer is discussed. It is used for structural analysis of single crystals on the basis of time-of-flight measurements. The diffractometer is positioned along the axis of a beam of the IBR-30 pulse reactor, its average power is 29 kW. The mechanical part of the diffractometer consists of a massive foundation with a threeaxial goniometer, a rotatable platform with a collimator and a 3 He counter. The flowsheet of a control unit is given, which is used to position the rotatable platform of the diffractometer. The control unit includes a 14 digic binary counter for rotation angle recording, a parallel-to-series converter, a control signal shaper, two position shift registers, and a servo mechanism. The accuracy of diffraction maxima is evaluated. It is found that the ratio D(t)sup(1/2)/t (D(t) is a time dispersion of diffraction maxima, t is total time-of-flight time), which characterize the resolution of the diffractometer, is equal to 0.5% at the Bragg angle Q=45 deg and the neutron wavelength Λ=1 A

  8. A Time of Flight Fast Neutron Imaging System Design Study

    Science.gov (United States)

    Canion, Bonnie; Glenn, Andrew; Sheets, Steven; Wurtz, Ron; Nakae, Les; Hausladen, Paul; McConchie, Seth; Blackston, Matthew; Fabris, Lorenzo; Newby, Jason

    2017-09-01

    LLNL and ORNL are designing an active/passive fast neutron imaging system that is flexible to non-ideal detector positioning. It is often not possible to move an inspection object in fieldable imager applications such as safeguards, arms control treaty verification, and emergency response. Particularly, we are interested in scenarios which inspectors do not have access to all sides of an inspection object, due to interfering objects or walls. This paper will present the results of a simulation-based design parameter study, that will determine the optimum system design parameters for a fieldable system to perform time-of-flight based imaging analysis. The imaging analysis is based on the use of an associated particle imaging deuterium-tritium (API DT) neutron generator to get the time-of-flight of radiation induced within an inspection object. This design study will investigate the optimum design parameters for such a system (e.g. detector size, ideal placement, etc.), as well as the upper and lower feasible design parameters that the system can expect to provide results within a reasonable amount of time (e.g. minimum/maximum detector efficiency, detector standoff, etc.). Ideally the final prototype from this project will be capable of using full-access techniques, such as transmission imaging, when the measurement circumstances allow, but with the additional capability of producing results at reduced accessibility.

  9. Characterization of modulated time-of-flight range image sensors

    Science.gov (United States)

    Payne, Andrew D.; Dorrington, Adrian A.; Cree, Michael J.; Carnegie, Dale A.

    2009-01-01

    A number of full field image sensors have been developed that are capable of simultaneously measuring intensity and distance (range) for every pixel in a given scene using an indirect time-of-flight measurement technique. A light source is intensity modulated at a frequency between 10-100 MHz, and an image sensor is modulated at the same frequency, synchronously sampling light reflected from objects in the scene (homodyne detection). The time of flight is manifested as a phase shift in the illumination modulation envelope, which can be determined from the sampled data simultaneously for each pixel in the scene. This paper presents a method of characterizing the high frequency modulation response of these image sensors, using a pico-second laser pulser. The characterization results allow the optimal operating parameters, such as the modulation frequency, to be identified in order to maximize the range measurement precision for a given sensor. A number of potential sources of error exist when using these sensors, including deficiencies in the modulation waveform shape, duty cycle, or phase, resulting in contamination of the resultant range data. From the characterization data these parameters can be identified and compensated for by modifying the sensor hardware or through post processing of the acquired range measurements.

  10. IceBridge Sigma Space Lidar L0 Raw Time-of-Flight Data

    Data.gov (United States)

    National Aeronautics and Space Administration — The NASA IceBridge Sigma Space Lidar L0 Raw Time-of-Flight Data (ILSIG0) contain raw time-of-flight values for Antarctica and Greenland using the Sigma Space Lidar....

  11. IPNS time-of-flight single crystal diffractometer

    International Nuclear Information System (INIS)

    Schultz, A.J.; Teller, R.G.; Williams, J.M.

    1983-01-01

    The single crystal diffractometer (SCD) at the Argonne Intense Pulsed Neutron Source (IPNS) utilizes the time-of-flight (TOF) Laue technique to provide a three-dimensional sampling of reciprocal space during each pulse. The instrument contains a unique neutron position-sensitive 6 Li-glass scintillation detector with an active area of 30 x 30 cm. The three-dimensional nature of the data is very useful for fast, efficient measurement of Bragg intensities and for the studies of superlattice and diffuse scattering. The instrument was designed to achieve a resolution of 2% or better (R = δQ/Q) with 2 THETA > 60 0 and lambda > 0.7A

  12. Avalanche photodiode based time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ogasawara, Keiichi, E-mail: kogasawara@swri.edu; Livi, Stefano A.; Desai, Mihir I.; Ebert, Robert W.; McComas, David J.; Walther, Brandon C. [Southwest Research Institute, 6220 Culebra Road, San Antonio, Texas 78238 (United States)

    2015-08-15

    This study reports on the performance of Avalanche Photodiodes (APDs) as a timing detector for ion Time-of-Flight (TOF) mass spectroscopy. We found that the fast signal carrier speed in a reach-through type APD enables an extremely short timescale response with a mass or energy independent <2 ns rise time for <200 keV ions (1−40 AMU) under proper bias voltage operations. When combined with a microchannel plate to detect start electron signals from an ultra-thin carbon foil, the APD comprises a novel TOF system that successfully operates with a <0.8 ns intrinsic timing resolution even using commercial off-the-shelf constant-fraction discriminators. By replacing conventional total-energy detectors in the TOF-Energy system, APDs offer significant power and mass savings or an anti-coincidence background rejection capability in future space instrumentation.

  13. High resolution fast neutron spectrometry without time-of-flight

    International Nuclear Information System (INIS)

    Evans, A.E.; Brandenberger, J.D.

    1978-01-01

    Performance tests of a spectrometer tube of the type developed by Cuttler and Shalev show that the measurement of fast neutron spectra with this device can be made with an energy resolution previously obtainable only in large time-of-flight facilities. In preliminary tests, resolutions of 16.4 keV for thermal neutrons and 30.9 keV for 1-MeV neutrons were obtained. A broad-window pulse-shape discrimination (PSD) system is used to remove from pulse-height distributions most of the continua due to 3 He-recoil events, noise, and wall effect. Use of PSD improved the energy resolution to 12.9 keV for thermal neutrons and 29.2 keV for 1-MeV neutrons. The detector is a viable tool for neutron research at nominally equipped accelerator laboratories

  14. Time Of Flight Detectors: From phototubes to SiPM

    International Nuclear Information System (INIS)

    Laurenti, G.; Levi, G.; Foschi, E.; Guandalini, C.; Quadrani, L.; Sbarra, C.; Zuffa, M.

    2008-01-01

    A sample of Silicon Photomultipliers was tested because they looked promising for future space missions: low consumption, low weight, resistance to radiation damage and insensitivity to magnetic fields. They have been studied in laboratory by means of the same characterization methods adopted to calibrate the fine mesh photomultipliers used by the Time Of Flight of the AMS-02 experiment. A detailed simulation was made to reproduce the SiPM response to the various experimental conditions. A possible counter design has been studied with front end electronics card equipped with SiPMs and Peltier cell for thermoregulation. A proper simulation based on COMSOL Multiphysics package reproduces quite well the Peltier cell nominal cooling capability

  15. Ultrasonic testing using time of flight diffraction technique (TOFD)

    International Nuclear Information System (INIS)

    Khurram Shahzad; Ahmad Mirza Safeer Ahmad; Muhammad Asif Khan

    2009-04-01

    This paper describes the ultrasonic testing using Time Flight Diffraction (TOFD) Technique for welded samples having different types and sizes of defects. TOFD is a computerized ultrasonic system, able to scan, store and evaluate indications in terms of location, through thickness and length in a more easy and convenient. Time of Flight Diffraction Technique (TOFD) is more fast and easy technique for ultrasonic testing as we can examine a weld i a single scan along the length of the weld with two probes known as D-scan. It shows the image of the complete weld with the defect information. The examinations were performed on carbon steel samples used for ultrasonic testing using 70 degree probes. The images for different type of defects were obtained. (author)

  16. Ion microtomography using ion time-of-flight

    International Nuclear Information System (INIS)

    Roberts, M.L.; Heikkinen, D.W.; Proctor, I.D.; Pontau, A.E.; Olona, G.T.; Felter, T.E.; Morse, D.H.; Hess, B.V.

    1992-01-01

    We have developed and are in the process of testing an ion time-of-flight (TOF) detector system for use in our ion microtomography measurements. Using TOF, ion energy is determined by measurement of the ion's flight time over a certain path length. For ion microtomography, the principle advantage of TOF analysis is that ion count rates of several hundred thousand counts per second can be achieved as compared to a limit of about ten thousand ions per second when using a solid-state silicon surface barrier detector and associated electronics. This greater than 10 fold increase in count rate correspondingly shortens sample analysis time or increases the amount of data that can be collected on a given sample. Details of the system and progress to date are described

  17. Tests and calibration of NIF neutron time of flight detectors.

    Science.gov (United States)

    Ali, Z A; Glebov, V Yu; Cruz, M; Duffy, T; Stoeckl, C; Roberts, S; Sangster, T C; Tommasini, R; Throop, A; Moran, M; Dauffy, L; Horsefield, C

    2008-10-01

    The National Ignition Facility (NIF) neutron time of flight (NTOF) diagnostic will measure neutron yield and ion temperature in all NIF campaigns in DD, DT, and THD(*) implosions. The NIF NTOF diagnostic is designed to measure neutron yield from 1x10(9) to 2x10(19). The NTOF consists of several detectors of varying sensitivity located on the NIF at about 5 and 20 m from the target. Production, testing, and calibration of the NIF NTOF detectors have begun at the Laboratory for Laser Energetics (LLE). Operational tests of the NTOF detectors were performed on several facilities including the OMEGA laser at LLE and the Titan laser at Lawrence Livermore National Laboratory. Neutron calibrations were carried out on the OMEGA laser. Results of the NTOF detector tests and calibration will be presented.

  18. Time-of-flight scattering and recoiling spectrometry

    International Nuclear Information System (INIS)

    Rabalais, J.W.

    1991-01-01

    Ion scattering and recoiling spectrometry consists of directing a collimated beam of monoenergetic ions towards a surface and measuring the flux of scattered and recoiled particles from this surface. When the neutral plus ion flux is velocity selected by measuring the flight times from the sample to the detector, the technique is called time-of-flight scattering and recoiling spectrometry (TOF-SARS). TOF-SARS is capable of (1) surface elemental analysis by applying classical mechanics to the velocities of the particles, (2) surface structural analysis by monitoring the angular anisotropies in the particle flux, and (3) ion-surface electron exchange probabilities by analysis of the ion/neutral fractions in the particle flux. Examples of these three areas are presented herein

  19. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    International Nuclear Information System (INIS)

    Cervera, M.I.; Beltran, J.; Lopez, F.J.; Hernandez, F.

    2011-01-01

    Highlights: → Employing a statistical optimization improves results reducing experiments. → Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. → Using Q/q intensity ratios is a powerful tool to ensure compound identification. → HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 μm fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 μg L -1 ). Recoveries between 70% and 120% were generally obtained with relative standard deviations (RSDs

  20. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Cervera, M.I. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Beltran, J., E-mail: joaquim.beltran@uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Lopez, F.J.; Hernandez, F. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

    2011-10-17

    Highlights: {yields} Employing a statistical optimization improves results reducing experiments. {yields} Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. {yields} Using Q/q intensity ratios is a powerful tool to ensure compound identification. {yields} HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 {mu}m fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 {mu}g L{sup -1}). Recoveries between 70% and 120% were generally obtained with

  1. Monoacylglycerol Analysis Using MS/MSALL Quadruple Time of Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Fei Gao

    2016-08-01

    Full Text Available Monoacylglycerols (MAGs are structural and bioactive metabolites critical for biological function. Development of facile tools for measuring MAG are essential to understand its role in different diseases and various pathways. A data-independent acquisition method, MS/MSALL, using electrospray ionization (ESI coupled quadrupole time of flight mass spectrometry (MS, was utilized for the structural identification and quantitative analysis of individual MAG molecular species. Compared with other acylglycerols, diacylglycerols (DAG and triacylglycerols (TAG, MAG characteristically presented as a dominant protonated ion, [M + H]+, and under low collision energy as fatty acid-like fragments due to the neutral loss of the glycerol head group. At low concentrations (<10 pmol/µL, where lipid-lipid interactions are rare, there was a strong linear correlation between ion abundance and MAG concentration. Moreover, using the MS/MSALL method the major MAG species from human plasma and mouse brown and white adipose tissues were quantified in less than 6 min. Collectively, these results demonstrate that MS/MSALL analysis of MAG is an enabling strategy for the direct identification and quantitative analysis of low level MAG species from biological samples with high throughput and sensitivity.

  2. Use of electron ionization and atmospheric pressure chemical ionization in gas chromatography coupled to time-of-flight mass spetrometry for screening and identification of organic pollutants in waters

    NARCIS (Netherlands)

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

    2014-01-01

    A new approach has been developed for multiclass screening of organic contaminants in water based on the use of gas chromatography coupled to hybrid quadrupole high-resolution time-of-flight mass spectrometry with atmospheric pressure chemical ionization (GC–(APCI)QTOF MS). The soft ionization

  3. Eddy covariance emission and deposition flux measurements using proton transfer reaction – time of flight – mass spectrometry (PTR-TOF-MS): comparison with PTR-MS measured vertical gradients and fluxes

    NARCIS (Netherlands)

    Park, J.H.; Goldstein, A.H.; Timkovsky, J|info:eu-repo/dai/nl/330541676; Fares, S.; Weber, R.; Karlik, J.; Holzinger, R.|info:eu-repo/dai/nl/337989338

    2013-01-01

    During summer 2010, a proton transfer reaction – time of flight – mass spectrometer (PTR-TOF-MS) and a quadrupole proton transfer reaction mass spectrometer (PTR-MS) were deployed simultaneously for one month in an orange orchard in the Central Valley of California to collect continuous data

  4. Time recording unit for a neutron time of flight spectrometer

    International Nuclear Information System (INIS)

    Puranik, Praful; Ajit Kiran, S.; Chandak, R.M.; Poudel, S.K.; Mukhopadhyay, R.

    2011-01-01

    Here the architecture and design of Time Recording Unit for a Neutron Time of Flight Spectrometer have been described. The Spectrometer would have an array of 50 Nos. of one meter long linear Position Sensitive Detector (PSD) placed vertically around the sample at a distance of 2000 mm. The sample receives periodic pulsed neutron beam coming through a Fermi chopper. The time and zone of detection of a scattered neutron in a PSD gives information of its flight time and path length, which will be used to calculate its energy. A neutron event zone (position) and time detection module for each PSD provides a 2 bit position/zone code and an event timing pulse. The path length assigned to a neutron detected in a zone (Z1, Z2 etc) in the PSD is the mean path length seen by the neutrons detected in that zone of the PSD. A Time recording unit described here receives event zone code and timing pulse for all the 50 detectors, tags a proper time window code to it, before streaming it to computer for calculation of the energy distribution of neutrons scattered from the sample

  5. Chern Numbers Hiding in Time of Flight Images

    Science.gov (United States)

    Satija, Indubala; Zhao, Erhai; Ghosh, Parag; Bray-Ali, Noah

    2011-03-01

    Since the experimental realization of synthetic magnetic fields in neural ultracold atoms, transport measurement such as quantized Hall conductivity remains an open challenge. Here we propose a novel and feasible scheme to measure the topological invariants, namely the chern numbers, in the time of flight images. We study both the commensurate and the incommensurate flux, with the later being the main focus here. The central concept underlying our proposal is the mapping between the chern numbers and the size of the dimerized states that emerge when the two-dimensional hopping is tuned to the highly anisotropic limit. In a uncoupled double quantum Hall system exhibiting time reversal invariance, only odd-sized dimer correlation functions are non-zero and hence encode quantized spin current. Finally, we illustrate that inspite of highly fragmented spectrum, a finite set of chern numbers are meaningful. Our results are supported by direct numerical computation of transverse conductivity. NBA acknowledges support from a National Research Council postdoctoral research associateship.

  6. Depth profiling of tritium by neutron time-of-flight

    International Nuclear Information System (INIS)

    Davis, J.C.; Anderson, J.D.; Lefevre, H.W.

    1976-01-01

    A method to measure the depth profile of tritium implanted or absorbed in materials was developed. The sample to be analyzed is bombarded with a pulsed proton beam and the energy of neutrons produced by the T(p,n) reaction is measured by the time-of-flight technique. From the neutron energy the depth in the target of the T atoms may be inferred. A sensitivity of 0.1 at. percent T or greater is possible. The technique is non-destructive and may be used with thick or radioactive host materials. Samples up to 20 μm in thickness may be profiled with resolution limited by straggling of the proton beam for depths greater than 1 μm. Deuterium depth profiling has been demonstrated using the D(d,n) reaction. The technique has been used to observe the behavior of an implantation spike of T produced by a 400 keV T + beam stopping at a depth of 3 μm in 11 μm thick layers of Ti and TiH. The presence of H in the Ti lattice is observed to inhibit the diffusion of T through the lattice. Effects of the total hydrogen concentration (H + T) being forced above stochiometry at the implantation site are suggested by the shapes of the implantation spikes

  7. Multiple-ion-beam time-of-flight mass spectrometer

    International Nuclear Information System (INIS)

    Rohrbacher, Andreas; Continetti, Robert E.

    2001-01-01

    An innovative approach to increase the throughput of mass spectrometric analyses using a multiple-ion-beam mass spectrometer is described. Two sample spots were applied onto a laser desorption/ionization target and each spot was simultaneously irradiated by a beam of quadrupled Nd:YLF laser radiation (261.75 nm) to produce ions by laser-desorption ionization. Acceleration of the ions in an electric field created parallel ion beams that were focused by two parallel einzel lens systems. After a flight path of 2.34 m, the ions were detected with a microchannel plate-phosphor screen assembly coupled with a charge coupled device camera that showed two resolved ion beams. Time-of-flight mass spectra were also obtained with this detector. Experiments were performed using both metal atom cations (Ti + and Cr + ) produced by laser desorption/ionization and the molecular ions of two different proteins (myoglobin and lysozyme), created by matrix assisted laser desorption/ionization using an excess of nicotinic acid as matrix

  8. Visualization of time-of-flight neutron diffraction data

    International Nuclear Information System (INIS)

    Mikkelson, D.J.; Price, D.L.; Worlton, T.G.

    1995-01-01

    The glass, liquids and amorphous materials diffractometer (GLAD) is a new instrument at the intense pulsed neutron source (IPNS) at Argonne National Laboratory. The GLAD currently has 218 linear position sensitive detectors arranged in five banks. Raw data collected from the instrument are typically split into 1000-1500 angular groups each of which contains approximately 2000 time channels. In order to obtain a meaningful overview of such a large amount of data, an interactive system to view the data has been designed. The system was implemented in C using the graphical kernel system (GKS) for portability.The system treats data from each bank of detectors as a three-dimensional data set with detector number, position along detector and time of flight as the three coordinate axes. The software then slices the data parallel to any of the coordinate planes and displays the slices as images. This approach has helped with the detailed analysis of detector electronics, verification of instrument calibration and resolution determination. In addition, it has helped to identify low-level background signals and provided insight into the overall operation of the instrument. ((orig.))

  9. Positron Emission Tomography (PET): Towards Time of Flight

    International Nuclear Information System (INIS)

    Karp, Joel

    2004-01-01

    PET is a powerful imaging tool that is being used to study cancer, using a variety of tracers to measure physiological processes including glucose metabolism, cell proliferation, and hypoxia in tumor cells. As the utilization of PET has grown in the last several years, it has become clear that improved lesion detection and quantification are critical goals for cancer studies. Although physical performance of the current generation of PET scanners has improved recently, there are limitations especially for heavy patients where attenuation and scatter effects are increased. We are investigating new scintillation detectors, scanner designs, and image processing algorithms in order to overcome these limitations and improve performance. In particular, we are studying scanner designs that would incorporate scintillators with improved energy and timing resolution. Improved energy resolution helps to reduce scattered radiation, and improved timing resolution makes it feasible to incorporate the time-of-flight information between the two coincident gamma rays into the image reconstruction algorithm, a technique that improves signal-to-noise. Results of recent experiments and computer simulations will be shown to demonstrate these potential improvements.

  10. Polarisation analysis on the LET time-of-flight spectrometer

    Science.gov (United States)

    Nilsen, G. J.; Košata, J.; Devonport, M.; Galsworthy, P.; Bewley, R. I.; Voneshen, D. J.; Dalgliesh, R.; Stewart, J. R.

    2017-06-01

    We present a design for implementing uniaxial polarisation analysis on the LET cold neutron time-of-flight spectrometer, installed on the second target station at ISIS. The polarised neutron beam is to be produced by a transmission-based supermirror polariser with the polarising mirrors arranged in a “double-V” formation. This will be followed by a Mezei-type precession coil spin flipper, selected for its small spatial requirements, as well as a permanent magnet guide field to transport the beam polarisation to the sample position. The sample area will contain a set of holding field coils, whose purpose is to produce a highly homogenous magnetic field for the wide-angle 3He analyser cell. To facilitate fast cell changes and reduce the risk of cell failure, we intend to separate the cell and cryostat from the vacuum of the sample tank by installing both in a vessel at atmospheric pressure. When the instrument upgrade is complete, the performance of LET is expected to be commensurate with existing and planned polarised cold neutron spectrometers at other sources. Finally, we discuss the implications of performing uniaxial polarisation analysis only, and identify quasi-elastic neutron scattering (QENS) on ionic conducting materials as an interesting area to apply the technique.

  11. Distance error correction for time-of-flight cameras

    Science.gov (United States)

    Fuersattel, Peter; Schaller, Christian; Maier, Andreas; Riess, Christian

    2017-06-01

    The measurement accuracy of time-of-flight cameras is limited due to properties of the scene and systematic errors. These errors can accumulate to multiple centimeters which may limit the applicability of these range sensors. In the past, different approaches have been proposed for improving the accuracy of these cameras. In this work, we propose a new method that improves two important aspects of the range calibration. First, we propose a new checkerboard which is augmented by a gray-level gradient. With this addition it becomes possible to capture the calibration features for intrinsic and distance calibration at the same time. The gradient strip allows to acquire a large amount of distance measurements for different surface reflectivities, which results in more meaningful training data. Second, we present multiple new features which are used as input to a random forest regressor. By using random regression forests, we circumvent the problem of finding an accurate model for the measurement error. During application, a correction value for each individual pixel is estimated with the trained forest based on a specifically tailored feature vector. With our approach the measurement error can be reduced by more than 40% for the Mesa SR4000 and by more than 30% for the Microsoft Kinect V2. In our evaluation we also investigate the impact of the individual forest parameters and illustrate the importance of the individual features.

  12. Towards time-of-flight PET with a semiconductor detector

    Science.gov (United States)

    Ariño-Estrada, Gerard; Mitchell, Gregory S.; Kwon, Sun Il; Du, Junwei; Kim, Hadong; Cirignano, Leonard J.; Shah, Kanai S.; Cherry, Simon R.

    2018-02-01

    The feasibility of using Cerenkov light, generated by energetic electrons following 511 keV photon interactions in the semiconductor TlBr, to obtain fast timing information for positron emission tomography (PET) was evaluated. Due to its high refractive index, TlBr is a relatively good Cerenkov radiator and with its wide bandgap, has good optical transparency across most of the visible spectrum. Coupling an SiPM photodetector to a slab of TlBr (TlBr-SiPM) yielded a coincidence timing resolution of 620 ps FWHM between the TlBr-SiPM detector and a LFS reference detector. This value improved to 430 ps FWHM by applying a high pulse amplitude cut based on the TlBr-SiPM and reference detector signal amplitudes. These results are the best ever achieved with a semiconductor PET detector and already approach the performance required for time-of-flight. As TlBr has higher stopping power and better energy resolution than the conventional scintillation detectors currently used in PET scanners, a hybrid TlBr-SiPM detector with fast timing capability becomes an interesting option for further development.

  13. Integrated intensities in inverse time-of-flight technique

    International Nuclear Information System (INIS)

    Dorner, Bruno

    2006-01-01

    In traditional data analysis a model function, convoluted with the resolution, is fitted to the measured data. In case that integrated intensities of signals are of main interest, one can use an approach which does not require a model function for the signal nor detailed knowledge of the resolution. For inverse TOF technique, this approach consists of two steps: (i) Normalisation of the measured spectrum with the help of a monitor, with 1/k sensitivity, which is positioned in front of the sample. This means at the same time a conversion of the data from time of flight to energy transfer. (ii) A Jacobian [I. Waller, P.O. Froeman, Ark. Phys. 4 (1952) 183] transforms data collected at constant scattering angle into data as if measured at constant momentum transfer Q. This Jacobian works correctly for signals which have a constant width at different Q along the trajectory of constant scattering angle. The approach has been tested on spectra of Compton scattering with neutrons, having epithermal energies, obtained on the inverse TOF spectrometer VESUVIO/ISIS. In this case the width of the signal is increasing proportional to Q and in consequence the application of the Jacobian leads to integrated intensities slightly too high. The resulting integrated intensities agree very well with results derived in the traditional way. Thus this completely different approach confirms the observation that signals from recoil by H-atoms at large momentum transfers are weaker than expected

  14. 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.

  15. The high-resolution time-of-flight spectrometer TOFTOF

    Energy Technology Data Exchange (ETDEWEB)

    Unruh, Tobias [Technische Universitaet Muenchen, Forschungsneutronenquelle Heinz Maier-Leibnitz FRM II and Physik Department E13, Lichtenbergstr. 1, 85747 Garching (Germany)], E-mail: Tobias.Unruh@frm2.tum.de; Neuhaus, Juergen; Petry, Winfried [Technische Universitaet Muenchen, Forschungsneutronenquelle Heinz Maier-Leibnitz FRM II and Physik Department E13, Lichtenbergstr. 1, 85747 Garching (Germany)

    2007-10-11

    The TOFTOF spectrometer is a multi-disc chopper time-of-flight spectrometer for cold neutrons at the research neutron source Heinz Maier-Leibnitz (FRM II). After five reactor cycles of routine operation the characteristics of the instrument are reported in this article. The spectrometer features an excellent signal to background ratio due to its remote position in the neutron guide hall, an elaborated shielding concept and an s-shaped curved primary neutron guide which acts i.a. as a neutron velocity filter. The spectrometer is fed with neutrons from the undermoderated cold neutron source of the FRM II leading to a total neutron flux of {approx}10{sup 10}n/cm{sup 2}/s in the continuous white beam at the sample position distributed over a continuous and particularly broad wavelength spectrum. A high energy resolution is achieved by the use of high speed chopper discs made of carbon-fiber-reinforced plastic. In the combination of intensity, resolution and signal to background ratio the spectrometer offers new scientific prospects in the fields of inelastic and quasielastic neutron scattering.

  16. The high-resolution time-of-flight spectrometer TOFTOF

    Science.gov (United States)

    Unruh, Tobias; Neuhaus, Jürgen; Petry, Winfried

    2007-10-01

    The TOFTOF spectrometer is a multi-disc chopper time-of-flight spectrometer for cold neutrons at the research neutron source Heinz Maier-Leibnitz (FRM II). After five reactor cycles of routine operation the characteristics of the instrument are reported in this article. The spectrometer features an excellent signal to background ratio due to its remote position in the neutron guide hall, an elaborated shielding concept and an s-shaped curved primary neutron guide which acts i.a. as a neutron velocity filter. The spectrometer is fed with neutrons from the undermoderated cold neutron source of the FRM II leading to a total neutron flux of ˜1010n/cm2/s in the continuous white beam at the sample position distributed over a continuous and particularly broad wavelength spectrum. A high energy resolution is achieved by the use of high speed chopper discs made of carbon-fiber-reinforced plastic. In the combination of intensity, resolution and signal to background ratio the spectrometer offers new scientific prospects in the fields of inelastic and quasielastic neutron scattering.

  17. Development of an ion time-of-flight spectrometer for neutron depth profiling

    Science.gov (United States)

    Cetiner, Mustafa Sacit

    signal. Without loss of generality, the secondary signal is obtained by the passage of the ion through a thin carbon foil, which produces ion-induced secondary electron emission (IISEE). The time-of-flight spectrometer physically acts as an ion/electron separator. The electrons that enter the active volume of the spectrometer are transported onto the microchannel plate detector to generate the secondary signal. The electron optics can be designed in variety of ways depending on the nature of the measurement and physical requirements. Two ion time-of-flight spectrometer designs are introduced: the parallel electric and magnetic (PEM) field spectrometer and the cross electric and magnetic (CEM) field spectrometer. The CEM field spectrometers have been extensively used in a wide range of applications where precise mass differentiation is required. The PEM field spectrometers have lately found interest in mass spectroscopy applications. The application of the PEM field spectrometer for energy measurements is a novel approach. The PEM field spectrometer used in the measurements employs axial electric and magnetic fields along the nominal direction of the incident ion. The secondary electrons are created by a thin carbon foil on the entrance disk and transported on the microchannel plate that faces the carbon foil. The initial angular distribution of the secondary electrons has virtually no effect on the transport time of the secondary electrons from the surface of the carbon foil to the electron microchannel plate detector. Therefore, the PEM field spectrometer can offer high-resolution energy measurement for relatively lower electric fields. The measurements with the PEM field spectrometer were made with the Tandem linear particle accelerator at the IBM T. J. Watson Research Center at Yorktown Heights, NY. The CEM field spectrometer developed for the thesis employs axial electric field along the nominal direction of the ion, and has perpendicular magnetic field. As the

  18. Recent developments in time-of-flight PET

    International Nuclear Information System (INIS)

    Vandenberghe, S.; Mikhaylova, E.; D’Hoe, E.; Mollet, P.; Karp, J. S.

    2016-01-01

    While the first time-of-flight (TOF)-positron emission tomography (PET) systems were already built in the early 1980s, limited clinical studies were acquired on these scanners. PET was still a research tool, and the available TOF-PET systems were experimental. Due to a combination of low stopping power and limited spatial resolution (caused by limited light output of the scintillators), these systems could not compete with bismuth germanate (BGO)-based PET scanners. Developments on TOF system were limited for about a decade but started again around 2000. The combination of fast photomultipliers, scintillators with high density, modern electronics, and faster computing power for image reconstruction have made it possible to introduce this principle in clinical TOF-PET systems. This paper reviews recent developments in system design, image reconstruction, corrections, and the potential in new applications for TOF-PET. After explaining the basic principles of time-of-flight, the difficulties in detector technology and electronics to obtain a good and stable timing resolution are shortly explained. The available clinical systems and prototypes under development are described in detail. The development of this type of PET scanner also requires modified image reconstruction with accurate modeling and correction methods. The additional dimension introduced by the time difference motivates a shift from sinogram- to listmode-based reconstruction. This reconstruction is however rather slow and therefore rebinning techniques specific for TOF data have been proposed. The main motivation for TOF-PET remains the large potential for image quality improvement and more accurate quantification for a given number of counts. The gain is related to the ratio of object size and spatial extent of the TOF kernel and is therefore particularly relevant for heavy patients, where image quality degrades significantly due to increased attenuation (low counts) and high scatter fractions. The

  19. LVGEMS Time-of-Flight Mass Spectrometry on Satellites

    Science.gov (United States)

    Herrero, Federico

    2013-01-01

    NASA fs investigations of the upper atmosphere and ionosphere require measurements of composition of the neutral air and ions. NASA is able to undertake these observations, but the instruments currently in use have their limitations. NASA has extended the scope of its research in the atmosphere and now requires more measurements covering more of the atmosphere. Out of this need, NASA developed multipoint measurements using miniaturized satellites, also called nanosatellites (e.g., CubeSats), that require a new generation of spectrometers that can fit into a 4 4 in. (.10 10 cm) cross-section in the upgraded satellites. Overall, the new mass spectrometer required for the new depth of atmospheric research must fulfill a new level of low-voltage/low-power requirements, smaller size, and less risk of magnetic contamination. The Low-Voltage Gated Electrostatic Mass Spectrometer (LVGEMS) was developed to fulfill these requirements. The LVGEMS offers a new spectrometer that eliminates magnetic field issues associated with magnetic sector mass spectrometers, reduces power, and is about 1/10 the size of previous instruments. LVGEMS employs the time of flight (TOF) technique in the GEMS mass spectrometer previously developed. However, like any TOF mass spectrometer, GEMS requires a rectangular waveform of large voltage amplitude, exceeding 100 V -- that means that the voltage applied to one of the GEMS electrodes has to change from 0 to 100 V in a time of only a few nanoseconds. Such electronic speed requires more power than can be provided in a CubeSat. In the LVGEMS, the amplitude of the rectangular waveform is reduced to about 1 V, compatible with digital electronics supplies and requiring little power.

  20. Time-of-flight PET image reconstruction using origin ensembles

    Science.gov (United States)

    Wülker, Christian; Sitek, Arkadiusz; Prevrhal, Sven

    2015-03-01

    The origin ensemble (OE) algorithm is a novel statistical method for minimum-mean-square-error (MMSE) reconstruction of emission tomography data. This method allows one to perform reconstruction entirely in the image domain, i.e. without the use of forward and backprojection operations. We have investigated the OE algorithm in the context of list-mode (LM) time-of-flight (TOF) PET reconstruction. In this paper, we provide a general introduction to MMSE reconstruction, and a statistically rigorous derivation of the OE algorithm. We show how to efficiently incorporate TOF information into the reconstruction process, and how to correct for random coincidences and scattered events. To examine the feasibility of LM-TOF MMSE reconstruction with the OE algorithm, we applied MMSE-OE and standard maximum-likelihood expectation-maximization (ML-EM) reconstruction to LM-TOF phantom data with a count number typically registered in clinical PET examinations. We analyzed the convergence behavior of the OE algorithm, and compared reconstruction time and image quality to that of the EM algorithm. In summary, during the reconstruction process, MMSE-OE contrast recovery (CRV) remained approximately the same, while background variability (BV) gradually decreased with an increasing number of OE iterations. The final MMSE-OE images exhibited lower BV and a slightly lower CRV than the corresponding ML-EM images. The reconstruction time of the OE algorithm was approximately 1.3 times longer. At the same time, the OE algorithm can inherently provide a comprehensive statistical characterization of the acquired data. This characterization can be utilized for further data processing, e.g. in kinetic analysis and image registration, making the OE algorithm a promising approach in a variety of applications.

  1. High-performance multiple-reflection time-of-flight mass spectrometers for research with exotic nuclei and for analytical mass spectrometry

    Science.gov (United States)

    Plaß, Wolfgang R.; Dickel, Timo; Ayet San Andres, Samuel; Ebert, Jens; Greiner, Florian; Hornung, Christine; Jesch, Christian; Lang, Johannes; Lippert, Wayne; Majoros, Tamas; Short, Devin; Geissel, Hans; Haettner, Emma; Reiter, Moritz P.; Rink, Ann-Kathrin; Scheidenberger, Christoph; Yavor, Mikhail I.

    2015-11-01

    A class of multiple-reflection time-of-flight mass spectrometers (MR-TOF-MSs) has been developed for research with exotic nuclei at present and future accelerator facilities such as GSI and FAIR (Darmstadt), and TRIUMF (Vancouver). They can perform highly accurate mass measurements of exotic nuclei, serve as high-resolution, high-capacity mass separators and be employed as diagnostics devices to monitor the production, separation and manipulation of beams of exotic nuclei. In addition, a mobile high-resolution MR-TOF-MS has been developed for in situ applications in analytical mass spectrometry ranging from environmental research to medicine. Recently, the MR-TOF-MS for GSI and FAIR has been further developed. A novel RF quadrupole-based ion beam switchyard has been developed that allows merging and splitting of ion beams as well as transport of ions into different directions. It efficiently connects a test and reference ion source and an auxiliary detector to the system. Due to an increase in the kinetic energy of the ions in the time-of-flight analyzer of the MR-TOF-MS, a given mass resolving power is now achieved in less than half the time-of-flight. Conversely, depending on the time-of-flight, the mass resolving power has been increased by a factor of more than two.

  2. Time-of-flight pulsed neutron diffraction of molten salts

    Energy Technology Data Exchange (ETDEWEB)

    Fukushima, Y; Misawa, M; Suzuki, K [Tohoku Univ., Sendai (Japan). Research Inst. for Iron, Steel and Other Metals

    1975-06-01

    In this work, the pulsed neutron diffraction of molten alkali metal nitrate and bismuth trihalide was measured by the time-of-flight method. An electron linear accelerator was used as the pulsed neutron source. All the measurements were carried out with the T-O-F neutron diffractometer installed on the 300 MeV electron lineac. Molten NaNO/sub 3/ and RbNO/sub 3/ were adopted as the samples for alkali metal nitrate. The measurement is in progress for KNO/sub 3/ and LiNO/sub 3/. As the first step of the study on bismuth-bismuth trihalide system, the temperature dependence of structure factors was observed for BiCl/sub 3/, BiBr/sub 3/ and BiI/sub 3/ in the liquid state. The structure factors Sm(Q) for molten NaNO/sub 3/ at 340/sup 0/C and RbNO/sub 3/ at 350/sup 0/C were obtained, and the form factor F/sub 1/(Q) for single NO/sub 3//sup -/ radical with equilateral triangle structure was calculated. In case of molten NaNO/sub 3/, the first peak of Sm(Q) is simply smooth and a small hump can be observed in the neighbourhood of the first minimum Q position. The first peak of Sm(Q) for molten RbNO/sub 3/ is divided into two peaks, whereas a hump at the first minimum becomes big, and shifts to the low Q side of the second peak. The size of the NO/sub 3//sup -/ radical in molten NaNO/sub 3/ is a little smaller than that in molten RbNO/sub 3/. The values of the bond length in the NO/sub 3//sup -/ radical are summarized for crystal state and liquid state. The temperature dependence of the structure factor S(Q) was observed for BiCl/sub 3/, BiBr/sub 3/ and BiI/sub 3/, and shown in a figure.

  3. Time-of-Flight Adjustment Procedure for Acoustic Measurements in Structural Timber

    Science.gov (United States)

    Danbiel F. Llana; Guillermo Iñiguez-Gonzalez; Francisco Arriaga; Xiping Wang

    2016-01-01

    The effect of timber length on time-of-flight acoustic longitudinal measurements was investigated on the structural timber of four Spanish species: radiata pine (Pinus radiata D. Don), Scots pine (Pinus sylvestris L.), laricio pine (Pinus nigra Arn.), and maritime pine (Pinus pinaster Ait.). Time-of-flight longitudinal measurements were conducted on 120 specimens of...

  4. ATLAS - analysis of time-of-flight diffraction data from liquid and amorphous samples

    International Nuclear Information System (INIS)

    Soper, A.K.; Howells, W.S.; Hannon, A.C.

    1989-05-01

    The purpose of this manual is to describe a package of data analysis routines which have been developed at the Rutherford Appleton Laboratory for the analysis of time-of-flight diffraction data from liquids, gases, and amorphous materials. There is no fundamental barrier to diffraction data being accurately analysed to structure factor or even pair correlation function within a very short time of the completion of the experiment. Section 1 describes the time-of-flight neutron diffraction experiment and looks at diffraction theory. Section 2 indicates the steps in data analysis of time-of-flight diffraction data and Section 3 gives details of how to run the procedures. (author)

  5. Time-of-flight experiments using a pseudo-statistical chopper

    International Nuclear Information System (INIS)

    Aizawa, Otohiko; Kanda, Keiji

    1975-01-01

    A ''pseudo-statistical'' chopper was manufactured and used for the experiments on neutron transmission and scattering. The characteristics of the chopper and the experimental results are discussed in comparison with those in the time-of-flight technique using a conventional chopper. Which of the two methods is superior depends on the form of the time-of-flight distribution to be measured. Pseudo-statistical pulsing may be especially advantageous for scattering experiments with single or a few-line time-of-flight spectrum. (auth.)

  6. Ion mobility analyzer - quadrupole mass spectrometer system design

    International Nuclear Information System (INIS)

    Cuna, C; Leuca, M; Lupsa, N; Mirel, V; Cuna, Stela; Cosma, V; Tusa, Florina; Bocos-Bintintan, V

    2009-01-01

    Because of their extremely high sensitivity for chemicals with elevated electronegativity or high proton affinity the ion mobility analysers are ideal for the ultra-trace detection of toxic or explosive chemicals, most of these situated often at concentration levels of sub-ppb (parts-per-billion). Ion mobility spectrometers (IMS) can be used to identify illicit drugs or environmental pollutants. Since resolution of an IMS is relatively low, to achieve an accurate identification of target analyte it is recommended to couple the IMS with a quadrupole mass spectrometer (QMS) or a time of flight mass spectrometer, acquiring in this way confirmatory information. This coupling is made through a specific interface. In this paper, an experimental model of such a tandem instrument, IMS-QMS is described. Accomplishment of this general purpose will be done, overcoming a series of specific issues. This implies the solving, using innovative solutions, of a series of complex issues: ensuring the stability of the ions beam generated by ion source; transfer with a good efficiency of the ionic current from IMS analyser to QMS; and realization of a special electronic circuitry which will be able to detect both positive and negative ions.

  7. Ion mobility analyzer - quadrupole mass spectrometer system design

    Energy Technology Data Exchange (ETDEWEB)

    Cuna, C; Leuca, M; Lupsa, N; Mirel, V; Cuna, Stela; Cosma, V; Tusa, Florina [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Bocos-Bintintan, V, E-mail: cornel.cuna@itim-cj.r [Babes-Bolyai University, Faculty of Environmental Sciences, 3 Fantanele, 400294 Cluj Napoca (Romania)

    2009-08-01

    Because of their extremely high sensitivity for chemicals with elevated electronegativity or high proton affinity the ion mobility analysers are ideal for the ultra-trace detection of toxic or explosive chemicals, most of these situated often at concentration levels of sub-ppb (parts-per-billion). Ion mobility spectrometers (IMS) can be used to identify illicit drugs or environmental pollutants. Since resolution of an IMS is relatively low, to achieve an accurate identification of target analyte it is recommended to couple the IMS with a quadrupole mass spectrometer (QMS) or a time of flight mass spectrometer, acquiring in this way confirmatory information. This coupling is made through a specific interface. In this paper, an experimental model of such a tandem instrument, IMS-QMS is described. Accomplishment of this general purpose will be done, overcoming a series of specific issues. This implies the solving, using innovative solutions, of a series of complex issues: ensuring the stability of the ions beam generated by ion source; transfer with a good efficiency of the ionic current from IMS analyser to QMS; and realization of a special electronic circuitry which will be able to detect both positive and negative ions.

  8. Physical design of time-of-flight mass spectrometer in energetic cluster impact deposition apparatus

    International Nuclear Information System (INIS)

    Yu Guoqing; Shi Ying; Chen Jingsheng; Zhu Dezhang; Pan Haochang; Xu Hongjie

    1999-01-01

    The principle and physical design of the time-of-flight mass spectrometer equipped in the energetic cluster impact deposition apparatus are introduced. Some problems existed in experiments and their solutions are also discussed

  9. Time-of-flight trigger based on the use of the time-to-amplitude converter

    International Nuclear Information System (INIS)

    Ladygin, V.P.; Man'yakov, P.K.; Reznikov, S.G.

    2000-01-01

    The method of the time-of-flight trigger realization based on the use of the time-to-amplitude converter is described. Such a trigger has a short decision time and high efficiency of the useful event selection. (author)

  10. Time-of-flight techniques applied to neutron spectra measurements in fast subcritical assemblies

    International Nuclear Information System (INIS)

    Rotival, Michel

    1975-04-01

    Time-of-flight measurements on Uranium-Graphite assemblies were performed using the BCMN linear accelerator. Methods to provide scalar spectra averaged over a core cell from these experimental results are described [fr

  11. Miniature Time of Flight Mass Spectrometer for Space and Extraterrestrial Applications, Phase II

    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...

  12. Single view reflectance capture using multiplexed scattering and time-of-flight imaging

    OpenAIRE

    Zhao, Shuang; Velten, Andreas; Raskar, Ramesh; Bala, Kavita; Naik, Nikhil Deepak

    2011-01-01

    This paper introduces the concept of time-of-flight reflectance estimation, and demonstrates a new technique that allows a camera to rapidly acquire reflectance properties of objects from a single view-point, over relatively long distances and without encircling equipment. We measure material properties by indirectly illuminating an object by a laser source, and observing its reflected light indirectly using a time-of-flight camera. The configuration collectively acquires dense angular, but l...

  13. Quantification of urinary 0,0'-dityrosine, a biomarker for oxidative damage to proteins, by high performance liquid chromatography with triple quadrupole tandem mas spectrometry. A comparison with ion-trap tandem mass spectrometry.

    NARCIS (Netherlands)

    Orhan, H.; Coolen, S.; Meerman, J.H.N.

    2005-01-01

    We recently described an isotope dilution reversed-phase liquid chromatography-atmospheric pressure chemical ionization-ion-trap-tandem mass spectrometry (HPLC-APCI-MS/MS) method for the quantitative determination of oxidized amino acids in human urine, including o,o′-dityrosine, a specific marker

  14. Recent advances of liquid chromatography-(tandem) mass spectrometry in clinical and forensic toxicology.

    Science.gov (United States)

    Peters, Frank T

    2011-01-01

    Liquid chromatography (LC) coupled to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) has become increasingly important in clinical and forensic toxicology as well as doping control and is now a robust and reliable technique for routine analysis in these fields. In recent years, methods for LC-MS(/MS)-based systematic toxicological analysis using triple quadrupole or ion trap instruments have been considerably improved and a new screening approach based on high-resolution MS analysis using benchtop time-of-flight MS instruments has been developed. Moreover, many applications for so-called multi-target screening and/or quantification of drugs, poisons, and or their metabolites in various biomatrices have been published. The present paper will provide an overview and discuss these recent developments focusing on the literature published after 2006. Copyright © 2010 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  15. Electrospray ionization tandem mass spectrometry of ammonium cationized polyethers.

    Science.gov (United States)

    Nasioudis, Andreas; Heeren, Ron M A; van Doormalen, Irene; de Wijs-Rot, Nicolette; van den Brink, Oscar F

    2011-05-01

    Quaternary ammonium salts (Quats) and amines are known to facilitate the MS analysis of high molar mass polyethers by forming low charge state adduct ions. The formation, stability, and behavior upon collision-induced dissociation (CID) of adduct ions of polyethers with a variety of Quats and amines were studied by electrospray ionization quadrupole time-of-flight, quadrupole ion trap, and linear ion trap tandem mass spectrometry (MS/MS). The linear ion trap instrument was part of an Orbitrap hybrid mass spectrometer that allowed accurate mass MS/MS measurements. The Quats and amines studied were of different degree of substitution, structure, and size. The stability of the adduct ions was related to the structure of the cation, especially the amine's degree of substitution. CID of singly/doubly charged primary and tertiary ammonium cationized polymers resulted in the neutral loss of the amine followed by fragmentation of the protonated product ions. The latter reveals information about the monomer unit, polymer sequence, and endgroup structure. In addition, the detection of product ions retaining the ammonium ion was observed. The predominant process in the CID of singly charged quaternary ammonium cationized polymers was cation detachment, whereas their doubly charged adduct ions provided the same information as the primary and tertiary ammonium cationized adduct ions. This study shows the potential of specific amines as tools for the structural elucidation of high molar mass polyethers. © American Society for Mass Spectrometry, 2011

  16. Determination of thyroid hormones in placenta using isotope-dilution liquid chromatography quadrupole time-of-flight mass spectrometry

    DEFF Research Database (Denmark)

    Li, Zhong-Min; Giesert, Florian; Vogt-Weisenhorn, Daniela

    2018-01-01

    The transplacental passage of thyroid hormones (THs) is of great significance since the maternal THs are vitally important in ensuring the normal fetal development. In this paper, we determined the concentrations of seven THs, viz. L-thyroxine (T4), 3,3',5-triiodo-l-thyronine (T3), 3,3',5'-triiod...

  17. [Separation and identification of bovine lactoferricin by high performance liquid chromatography-matrix-assisted laser desorption/ionization time of flight/ time of flight mass spectrometry].

    Science.gov (United States)

    An, Meichen; Liu, Ning

    2010-02-01

    A high performance liquid chromatography-matrix-assisted laser desorption/ionization time of flight/time of flight mass spectrometry (HPLC-MALDI-TOF/TOF MS) method was developed for the separation and identification of bovine lactoferricin (LfcinB). Bovine lactoferrin was hydrolyzed by pepsin and then separated by ion exchange chromatography and reversed-phase liquid chromatography (RP-LC). The antibacterial activities of the fractions from RP-LC separation were determined and the protein concentration of the fraction with the highest activity was measured, whose sequence was indentified by MALDI-TOF/TOF MS. The relative molecular mass of LfcinB was 3 124.89 and the protein concentration was 18.20 microg/mL. The method of producing LfcinB proposed in this study has fast speed, high accuracy and high resolution.

  18. Application of high-performance liquid chromatography-tandem mass spectrometry with a quadrupole/linear ion trap instrument for the analysis of pesticide residues in olive oil.

    Science.gov (United States)

    Hernando, M D; Ferrer, C; Ulaszewska, M; García-Reyes, J F; Molina-Díaz, A; Fernández-Alba, A R

    2007-11-01

    This article describes the development of an enhanced liquid chromatography-mass spectrometry (LC-MS) method for the analysis of pesticides in olive oil. One hundred pesticides belonging to different classes and that are currently used in agriculture have been included in this method. The LC-MS method was developed using a hybrid quadrupole/linear ion trap (QqQ(LIT)) analyzer. Key features of this technique are the rapid scan acquisition times, high specificity and high sensitivity it enables when the multiple reaction monitoring (MRM) mode or the linear ion-trap operational mode is employed. The application of 5 ms dwell times using a linearly accelerating (LINAC) high-pressure collision cell enabled the analysis of a high number of pesticides, with enough data points acquired for optimal peak definition in MRM operation mode and for satisfactory quantitative determinations to be made. The method quantifies over a linear dynamic range of LOQs (0.03-10 microg kg(-1)) up to 500 microg kg(-1). Matrix effects were evaluated by comparing the slopes of matrix-matched and solvent-based calibration curves. Weak suppression or enhancement of signals was observed (ion (EPI) and MS3 were developed.

  19. Assessing and minimizing contamination in time of flight based validation data

    Science.gov (United States)

    Lennox, Kristin P.; Rosenfield, Paul; Blair, Brenton; Kaplan, Alan; Ruz, Jaime; Glenn, Andrew; Wurtz, Ronald

    2017-10-01

    Time of flight experiments are the gold standard method for generating labeled training and testing data for the neutron/gamma pulse shape discrimination problem. As the popularity of supervised classification methods increases in this field, there will also be increasing reliance on time of flight data for algorithm development and evaluation. However, time of flight experiments are subject to various sources of contamination that lead to neutron and gamma pulses being mislabeled. Such labeling errors have a detrimental effect on classification algorithm training and testing, and should therefore be minimized. This paper presents a method for identifying minimally contaminated data sets from time of flight experiments and estimating the residual contamination rate. This method leverages statistical models describing neutron and gamma travel time distributions and is easily implemented using existing statistical software. The method produces a set of optimal intervals that balance the trade-off between interval size and nuisance particle contamination, and its use is demonstrated on a time of flight data set for Cf-252. The particular properties of the optimal intervals for the demonstration data are explored in detail.

  20. Development of a multiresidue method for the determination of endocrine disrupters in fish fillet using gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Munaretto, Juliana S; Ferronato, Giovana; Ribeiro, Lucila C; Martins, Manoel L; Adaime, Martha B; Zanella, Renato

    2013-11-15

    Endocrine Disrupter Compounds (EDCs) are responsible for alterations in the endocrine system functions. Aquatic organisms are able to accumulate EDCs residues, being the major source of contamination for top predators and human consumers. This study aimed to develop and validate a method for the determination of 40 EDCs in fish fillet using modified QuEChERS and Gas Chromatography coupled with Mass Spectrometry in tandem (GC-MS/MS). A factorial design was used to optimize the extraction procedure. Method validation presented recoveries from 70.1% to 120.0% with RSDfish fillet from different species and residues of bisphenol A, chlorpyrifos and bifenthrin were detected. The proposed method proved to be effective for the determination of EDCs in fish fillet at very low concentration levels. © 2013 Elsevier B.V. All rights reserved.

  1. Applicability of Gas Chromatography (GC) Coupled to Triple-Quadrupole (QqQ) Tandem Mass Spectrometry (MS/MS) for Polybrominated Diphenyl Ether (PBDE) and Emerging Brominated Flame Retardant (BFR) Determinations in Functional Foods Enriched in Omega-3.

    Science.gov (United States)

    García-Bermejo, Ángel; Mohr, Susana; Herrero, Laura; González, María-José; Gómara, Belén

    2016-09-28

    This paper reports on the optimization, characterization, and applicability of gas chromatography coupled to triple-quadrupole tandem mass spectrometry (GC-QqQ(MS/MS)) for the determination of 14 polybrominated diphenylethers (PBDEs) and 2 emerging brominated flame retardants, 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) and decabromodiphenylethane (DBDPE), in functional food samples. The method showed satisfactory precision and linearity with instrumental limits of detection (iLODs) ranging from 0.12 to 7.1 pg, for tri- to octa-BDEs and BTBPE, and equal to 51 and 20 pg for BDE-209 and DBDPE, respectively. The highest ΣBFR concentrations were found in fish oil supplements (924 pg/g fresh weight, fw), followed by biscuits (90 pg/g fw), vegetable oil supplements (46 pg/g fw), chicken eggs (45 pg/g fw), cow's milk (7.7 pg/g fw), and soy products (1.6 pg/g fw). BDE-47, BDE-99, and DBDPE were the most abundant compounds. Foodstuffs enriched with omega-3 presented concentrations similar to or even lower than those of conventional foods commercialized in Spain since 2000.

  2. A Time-of-Flight System for Low Energy Charged Particles

    Science.gov (United States)

    Giordano, Micheal; Sadwick, Krystalyn; Fletcher, Kurt; Padalino, Stephen

    2013-10-01

    A time-of-flight system has been developed to measure the energy of charged particles in the keV range. Positively charged ions passing through very thin carbon films mounted on grids generate secondary electrons. These electrons are accelerated by a -2000 V grid bias towards a grounded channeltron electron multiplier (CEM) which amplifies the signal. Two CEM detector assemblies are mounted 23.1 cm apart along the path of the ions. An ion generates a start signal by passing through the first CEM and a stop signal by passing through the second. The start and stop signals generate a time-of-flight spectrum via conventional electronics. Higher energy alpha particles from radioactive sources have been used to test the system. This time-of-flight system will be deployed to measure the energies of 15 to 30 keV ions produced by a duoplasmatron ion source that is used to characterize ICF detectors.

  3. Multi-residue analysis of legacy POPs and emerging organic contaminants in Singapore's coastal waters using gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Hui; Bayen, Stéphane; Kelly, Barry C

    2015-08-01

    A gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) based method was developed for determination of 86 hydrophobic organic compounds in seawater. Solid-phase extraction (SPE) was employed for sequestration of target analytes in the dissolved phase. Ultrasound assisted extraction (UAE) and florisil chromatography were utilized for determination of concentrations in suspended sediments (particulate phase). The target compounds included multi-class hydrophobic contaminants with a wide range of physical-chemical properties. This list includes several polycyclic and nitro-aromatic musks, brominated and chlorinated flame retardants, methyl triclosan, chlorobenzenes, organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs). Spiked MilliQ water and seawater samples were used to evaluate the method performance. Analyte recoveries were generally good, with the exception of some of the more volatile target analytes (chlorobenzenes and bromobenzenes). The method is very sensitive, with method detection limits typically in the low parts per quadrillion (ppq) range. Analysis of 51 field-collected seawater samples (dissolved and particulate-bound phases) from four distinct coastal sites around Singapore showed trace detection of several polychlorinated biphenyl congeners and other legacy POPs, as well as several current-use emerging organic contaminants (EOCs). Polycyclic and nitro-aromatic musks, bromobenzenes, dechlorane plus isomers (syn-DP, anti-DP) and methyl triclosan were frequently detected at appreciable levels (2-20,000pgL(-1)). The observed concentrations of the monitored contaminants in Singapore's marine environment were generally comparable to previously reported levels in other coastal marine systems. To our knowledge, these are the first measurements of these emerging contaminants of concern in Singapore or Southeast Asia. The developed method may prove beneficial for future environmental monitoring of hydrophobic organic contaminants

  4. Potential advantages of a cesium fluoride scintillator for a time-of-flight positron camera

    International Nuclear Information System (INIS)

    Allemand, R.; Gresset, C.; Vacher, J.

    1980-01-01

    In order to improve the quality of positron tomographic imaging, a time-of-flight technique combined with a classical reconstruction method has been investigated. The decay time of NaI(Tl) and bismuth germanate (BGO) scintillators is too long for this application, and efficiency of the plastic scintillators is too low. Cesium fluoride appears to be a very promising detector material. This paper presents preliminary results obtained with a time-of-flight technique using CsF scintillators. The expected advantages were realized

  5. The Dynamic Method for Time-of-Flight Measurement of Thermal Neutron Spectra from Pulsed Sources

    International Nuclear Information System (INIS)

    Pepelyshev, Yu.N.; Tulaev, A.B.; Bobrakov, V.F.

    1994-01-01

    The time-of-flight method for a measurement of thermal neutron spectra in the pulsed neutron sources with high efficiency of neutron registration, more than 10 5 times higher in comparison with traditional one, is described. The main problems connected with the electric current technique for time-of-flight spectra measurement are examined. The methodical errors, problems of a special neutron detector design and other questions are discussed. Some experimental results, spectra from surfaces of the water and solid methane moderators, obtained in the pulsed reactor IBR-2 (Dubna, Russia) are presented. 4 refs., 5 figs

  6. Comparison of detector materials for time-of-flight positron tomography

    International Nuclear Information System (INIS)

    Derenzo, S.E.

    1982-06-01

    Knowledge of detection efficiency and timing resolution is essential when comparing detector materials for time-of-flight positron tomography. We present results of Monte Carlo calculations of the detection efficiency of plastic, lead loaded plastic, NaI(T1), liquid xenon, bismuth germanate (BGO), CsF, BaF 2 , Ge, and HgI 2 for 511 keV photons. We also use recently published values of timing resolution for these detector materials to tabulate the quantity (efficiency) 2 /(time resolution) which is a measure of the relative sensitivity for time of flight positron tomography

  7. Design, construction, characterization, and use of a detector to measure time of flight of cosmic rays

    Science.gov (United States)

    Araujo, A. C.; Felix, J.

    2017-01-01

    In the study of cosmic rays, measurements of time of flight and momentum have been used to identify incident particles from its physical properties, like mass. In this document we present the design, construction, characterization, and operation of a detector to measure time of flight of cosmic rays. The device is comprised of three small plates of plastic scintillator arranged in vertical straight line, coupled to one photomultiplier tube. The analogical output has been connected to a data acquisition system to obtain the number of digital pulses per millisecond. We present details of design, construction, operation, and preliminary results.

  8. The dynamic method for time-of-flight measurement of thermal neutron spectra from pulsed sources

    International Nuclear Information System (INIS)

    Pepyolyshev, Yu.N.; Chuklyaev, S.V.; Tulaev, A.B.; Bobrakov, V.F.

    1995-01-01

    A time-of-flight method for measurement of thermal neutron spectra in pulsed neutron sources with an efficiency more than 10 5 times higher than the standard method is described. The main problems associated with the electric current technique for time-of-flight spectra measurement are examined. The methodical errors, problems of special neutron detector design and other questions are discussed. Some experimental results for spectra from the surfaces of water and solid methane moderators obtained at the IBR-2 pulsed reactor (Dubna, Russia) are presented. (orig.)

  9. Simultaneous Determination of Fifteen Constituents of Jitai Tablet Using Ultra High-Performance Liquid Chromatography Coupled with Triple Quadrupole Electrospray Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Shuping Wang

    2014-01-01

    Full Text Available An ultra-high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS method was developed for simultaneous determination of fifteen constituents in Jitai tablet (JTT, a complex Traditional Chinese Medicine prescription (TCMP used in treating opiate addiction. Benefitting from a small particle size (1.8 µm C18 column, accelerated analysis with satisfactory resolution, sensitivity and selectivity were achieved in a single run within 7 min with linear gradient elution of acetonitrile-0.1% (v/v formic acid in water. The analytical signal was obtained by multiple reaction monitoring transitions via electrospray ionization source operating in both positive and negative ionization mode. The approach was validated for linearity, sensitivity, precision, repeatability, stability and recovery. All analytes showed good linearity over a wide concentration range (r > 0.99. The method limits ranged from 0.03 ng/mL to 19.35 ng/mL which are sensitive enough for quality control studies. The developed method was successfully applied to the simultaneous determination of fifteen constituents in JTT. In conclusion, our experimental results demonstrate that UHPLC-ESI-MS/MS is a useful approach for the overall quality assessment of complex TCMPs.

  10. Quantitative analysis of the major constituents in Chinese medicinal preparation SuoQuan formulae by ultra fast high performance liquid chromatography/quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Chen, Feng; Li, Hai-Long; Li, Yong-Hui; Tan, Yin-Feng; Zhang, Jun-Qing

    2013-07-30

    The SuoQuan formulae containing Fructus Alpiniae Oxyphyllae has been used to combat the urinary incontinence symptoms including frequency, urgency and nocturia for hundreds of years in China. However, the chemical information was not well characterized. The quality control marker constituent only focused on one single compound in the current Chinese Pharmacopeia. Hence it is prudent to identify and quantify the main constituents in this herbal product. This study aimed to analyze the main constituents using ultra-fast performance liquid chromatography coupled to tandem mass spectrometry (UFLC-MS/MS). Fourteen phytochemicals originated from five chemical classes constituents were identified by comparing the molecular mass, fragmentation pattern and retention time with those of the reference standards. A newly developed UFLC-MS/MS was validated demonstrating that the new assay was valid, reproducible and reliable. This method was successfully applied to simultaneously quantify the fourteen phytochemicals. Notably, the content of these constituents showed significant differences in three pharmaceutical preparations. The major constituent originated from each of chemical class was isolinderalactone, norisoboldine, nootkatone, yakuchinone A and apigenin-4',7-dimethylther, respectively. The variation among these compounds was more than 1000 times. Furthermore, the significant content variation between the two different Suoquan pills was also observed. The proposed method is sensitive and reliable; hence it can be used to analyze a variety of SuoQuan formulae products produced by different pharmaceutical manufacturers.

  11. Ultra-fast liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry for the rapid phenolic profiling of red maple (Acer rubrum) leaves.

    Science.gov (United States)

    Li, Chunting; Seeram, Navindra P

    2018-03-07

    The red maple (Acer rubrum) species is economically important to North America because of its sap, which is used to produce maple syrup. In addition, various other red maple plant parts, including leaves, were used as a traditional medicine by the Native Americans. Currently, red maple leaves are being used for nutraceutical and cosmetic applications but there are no published analytical methods for comprehensive phytochemical characterization of this material. Herein, a rapid and sensitive method using liquid chromatography with electrospray ionization time-of-flight tandem mass spectrometry was developed to characterize the phenolics in a methanol extract of red maple leaves and a proprietary phenolic-enriched red maple leaves extract (Maplifa™). Time-of-flight mass spectrometry and tandem mass spectrometry experiments led to the identification of 106 phenolic compounds in red maples leaves with the vast majority of these compounds also detected in Maplifa™. The compounds included 68 gallotannins, 25 flavonoids, gallic acid, quinic acid, catechin, epicatechin, and nine other gallic acid derivatives among which 11 are potentially new and 75 are being reported from red maple for the first time. The developed method to characterize red maple leaves phenolics is rapid and highly sensitive and could aid in future standardization and quality control of this botanical ingredient. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Time-of-Flight Measurement of the Speed of Sound in a Metal Bar

    Science.gov (United States)

    Ganci, Salvatore

    2016-01-01

    A simple setup was designed for a "time-of-flight" measurement of the sound speed in a metal bar. The experiment requires low cost components and is very simple to understand by students. A good use of it is as a demonstration experiment.

  13. Computer-controlled neutron time-of-flight spectrometer. Part II

    International Nuclear Information System (INIS)

    Merriman, S.H.

    1979-12-01

    A time-of-flight spectrometer for neutron inelastic scattering research has been interfaced to a PDP-15/30 computer. The computer is used for experimental data acquisition and analysis and for apparatus control. This report was prepared to summarize the functions of the computer and to act as a users' guide to the software system

  14. Four-Spot Time-Of-Flight Laser Anemometer For Turbomachinery

    Science.gov (United States)

    Wernet, Mark P.; Skoch, Gary J.

    1995-01-01

    Two-color, four-spot time-of-flight laser anemometer designed for measuring flow velocity within narrow confines of small centrifugal compressor. Apparatus well suited for measuring fast (typical speeds 160 to 700 m/s), highly turbulent gas flows in turbomachinery. Other potential applications include measurement of gas flows in pipelines and in flows from explosions.

  15. TOF-SEMSANS—Time-of-flight spin-echo modulated small-angle neutron scattering

    NARCIS (Netherlands)

    Strobl, M.; Tremsin, A.S.; Hilger, A.; Wieder, F.; Kardjilov, N.; Manke, I.; Bouwman, W.G.; Plomp, J.

    2012-01-01

    We report on measurements of spatial beam modulation of a polarized neutron beam induced by triangular precession regions in time-of-flight mode and the application of this novel technique spin-echo modulated small-angle neutron scattering (SEMSANS) to small-angle neutron scattering in the very

  16. Residual stress analysis by neutron time-of-flight at a reactor source

    International Nuclear Information System (INIS)

    Priesmeyer, H.G.; Schroder, J.

    1990-01-01

    Non-destructive neutron diffractometry for stress analysis will be a powerful experimental tool in material science research performed at the GKSS 5 MW reactor FRG-1. Arguments which show the advantages of the time-of-flight method are given and a suitable high-resolution neutron-efficient type of spectrometer is introduced. First results derived from this method are presented

  17. WINTOF - A program to produce neutron spectra from Zebra time-of-flight experiments

    International Nuclear Information System (INIS)

    Marshall, J.

    1969-06-01

    This report describes a computer program, written for the Winfrith KDF9 computer, which is used to calculate the neutron energy spectrum in the Zebra reactor from neutron time-of-flight measurements using the Zebra Linac. The data requirements for the program are specified and an illustration of the final spectrum is included. (author)

  18. FOCUS: neutron time-of-flight spectrometer at SINQ: recent progress

    Energy Technology Data Exchange (ETDEWEB)

    Janssen, S.; Mesot, J.; Holitzner, L. [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Hempelmann, R. [Saarbruecken Univ. (Germany)

    1997-09-01

    At the Swiss neutron spallation source SINQ a time-of-flight spectrometer for cold neutrons is under construction. The design foresees a Hybrid solution combining a Fermi chopper with a doubly focusing crystal monochromator. During 1996 important progress has been made concerning the main spectrometer components such as the spectrometer housing and the detector system. (author) 2 figs., 3 refs.

  19. Computationally effective solution of the inverse problem in time-of-flight spectroscopy

    DEFF Research Database (Denmark)

    Kamran, Faisal; Abildgaard, Otto Højager Attermann; Subash, Arman Ahamed

    2015-01-01

    Photon time-of-flight (PTOF) spectroscopy enables the estimation of absorption and reduced scattering coefficients of turbid media by measuring the propagation time of short light pulses through turbid medium. The present investigation provides a comparison of the assessed absorption and reduced...

  20. Incident spectrum determination for time-of-flight neutron powder diffraction data analysis

    International Nuclear Information System (INIS)

    Hodges, J. P.

    1998-01-01

    Accurate characterization of the incident neutron spectrum is an important requirement for precise Rietveld analysis of time-of-flight powder neutron diffraction data. Without an accurate incident spectrum the calculated model for the measured relative intensities of individual Bragg reflections will possess systematic errors. We describe a method for obtaining an accurate numerical incident spectrum using data from a transmitted beam monitor

  1. arXiv Performance of the ALICE Time-Of-Flight detector at the LHC

    CERN Document Server

    INSPIRE-00531272

    The ALICE Time-Of-Flight (TOF) detector at LHC is based on the Multigap Resistive Plate Chambers (MRPCs). The TOF performance during LHC Run 2 is here reported. Particular attention is given to the improved time resolution reached by TOF detector of $56$ ps, with the consequently improved particle identification capabilities.

  2. Proceedings of the 1986 workshop on advanced time-of-flight neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lawson, A.C.; Smith, K. (comps.)

    1986-09-01

    This report contains abstracts of talks and summaries of discussions from a small workshop held to discuss the future of time-of-flight neutron powder diffraction and its implementation at the Los Alamos Neutron Scattering Center. 47 refs., 3 figs.

  3. Experiments at the time-of-flight neutron spectrometer GNEIS in Gatchina

    International Nuclear Information System (INIS)

    Shcherbakov, O.A.

    1990-01-01

    A brief description of the Gatchina neutron time-of-flight spectrometer GNEIS at the 1 GeV proton synchrocyclotron and its main characteristics are given. Some results of the nuclear fission experiments and neutron cross section measurements are presented not only to illustrate the facility performance but to outline the basic directions of the researches as well. 28 refs.; 10 figs

  4. A fast preamplifier concept for SiPM-based time-of-flight PET detectors

    NARCIS (Netherlands)

    Huizenga, J.; Seifert, S.; Schreuder, F.; Dendooven, P.; Löhner, H.; Vinke, R.; Schaart, D. R.; van Dam, H.T.

    2012-01-01

    Silicon photomultipliers (SiPMs) offer high gain and fast response to light, making them interesting for fast timing applications such as time-of-flight (TOF) PET. To fully exploit the potential of these photosensors, dedicated preamplifiers that do not deteriorate the rise time and signal-to-noise

  5. Sub-nanosecond time-of-flight for segmented silicon detectors

    International Nuclear Information System (INIS)

    Souza, R.T. de; Alexander, A.; Brown, K.; Floyd, B.; Gosser, Z.Q.; Hudan, S.; Poehlman, J.; Rudolph, M.J.

    2011-01-01

    Development of a multichannel time-of-flight system for readout of a segmented, ion-passivated, ion-implanted silicon detector is described. This system provides sub-nanosecond resolution (δt∼370ps) even for low energy α particles which deposit E≤7.687MeV in the detector.

  6. Plant Leaf Imaging using Time of Flight Camera under Sunlight, Shadow and Room Conditions

    DEFF Research Database (Denmark)

    Kazmi, Wajahat; Foix, Sergi; Alenya, Guillem

    2012-01-01

    In this article, we analyze the effects of ambient light on Time of Flight (ToF) depth imaging for a plant's leaf in sunlight, shadow and room conditions. ToF imaging is sensitive to ambient light and we try to find the best possible integration times (IT) for each condition. This is important in...

  7. Processing of acquisition data for a time of flight positron tomograph

    International Nuclear Information System (INIS)

    Robert, G.

    1987-10-01

    After a review of basic principles concerning the time of flight positron tomography, the LETI positron tomograph is briefly described. For performance optimization (acquisition, calibration, image reconstruction), various specialized operators have been designed: the realization of the acquisition system is presented [fr

  8. Analysis of gait using a treadmill and a Time-of-flight camera

    DEFF Research Database (Denmark)

    Jensen, Rasmus Ramsbøl; Paulsen, Rasmus Reinhold; Larsen, Rasmus

    2009-01-01

    We present a system that analyzes human gait using a treadmill and a Time-of-flight camera. The camera provides spatial data with local intensity measures of the scene, and data are collected over several gait cycles. These data are then used to model and analyze the gait. For each frame...

  9. Proceedings of the 1986 workshop on advanced time-of-flight neutron powder diffraction

    International Nuclear Information System (INIS)

    Lawson, A.C.; Smith, K.

    1986-09-01

    This report contains abstracts of talks and summaries of discussions from a small workshop held to discuss the future of time-of-flight neutron powder diffraction and its implementation at the Los Alamos Neutron Scattering Center. 47 refs., 3 figs

  10. Data acquisition system for a positron tomograph using time-of-flight information

    International Nuclear Information System (INIS)

    Bertin, Francois.

    1981-12-01

    Progress in nuclear instrumentation has led to the development of scintillators much faster than the NaI crystal traditionally used in nuclear medicine. As a result it is now possible to measure time-of-flight, i.e. the time between the arrival of two γ rays emitted in coincidence on two detectors. With this extra information the β + annihilation site may be located. The introduction of time-of-flight in tomographic techniques called for research along two lines: - ''theoretical'' research leading to the creation of a new image reconstruction algorithm taking into account time-of-flight information - applied research leading to the development of an efficient measurement line and sophisticated data acquisition and processing electronics. This research has been carried out at LETI and is briefly outlined in chapter I. Chapter II shows how the introduction of time-of-flight and the modification of the reconstruction algorithm complicate the electronic and informatic equipment of the tomograph. Several acquisition and processing strategies are proposed, then the need to use an intermediate mass storage and hence to design a complex acquisition operator is demonstrated. Chapter III examines the structure of the acquisition operator and the resulting block diagram is presented in detail in chapter IV [fr

  11. BGO as a hybrid scintillator / Cherenkov radiator for cost-effective time-of-flight PET

    NARCIS (Netherlands)

    Brunner, S.E.K.; Schaart, D.R.

    2017-01-01

    Due to detector developments in the last decade, the time-of-flight (TOF) method is now commonly used to improve the quality of positron emission tomography (PET) images. Clinical TOF-PET systems based on L(Y)SO:Ce crystals and silicon photomultipliers (SiPMs) with coincidence resolving times

  12. A position-sensitive start detector for time-of-flight measurement

    International Nuclear Information System (INIS)

    Ikezoe, Hiroshi; Shikazono, Naomoto; Isoyama, Goro.

    1978-08-01

    A position-sensitive start detector for a time-of-flight measurement is described. In this detector microchannel plates were used to obtain time and position signals simultaneously. A time resolution of 121 psec FWHM and a position resolution of 0.28 mm FWHM were obtained for α-particles from an 241 Am source. (auth.)

  13. Time of flight diffraction technique and applications for retaining rings and turbine discs

    International Nuclear Information System (INIS)

    Ashwin, P.

    1990-01-01

    During recent times the term Time of Flight has become a popular phrase in ultrasonic terminology. It is true to say that since ultrasonic energy was first applied for NDE applications, we have used the time of flight to measure the material thickness and establish the presence of discontinuities in metals and other materials. However, as digital ultrasonic systems have evolved we have added new terminology to the field of nondestructive testing, such that phrases as Time of Flight are often misunderstood or over used. Conventional ultrasonic practice (meaning code based ultrasonic inspection) is in most reliant on the measurement of the reflected amplitude response to establish the presence and size of material discontinuities, where the time of flight is the measurement of the ultrasound as it travels to and from the reflector. This industry standard technique has on many occasions been questioned in terms of its value, especially during defect sizing applications. To address the known limitations of amplitude based sizing criteria, a new technique was developed referred to as Time Of Flight Diffraction -TOFD. Instead of using the amount of ultrasonic energy reflected by a discontinuity, TOFD relies on an aspect of ultrasonics that until more recently has been ignored or overlooked. This is the phenomena of diffracted ultrasonic energy, Using diffracted energy it is possible to more accurately measure the size of a defect. More recently the technique has been used for the detection of defects, where due to the imaging capabilities of the instrumentation used, TOFD has illustrated the presence of defects which could not be identified by other ultrasonic methods

  14. Qualitative and Quantitative Analysis of Andrographis paniculata by Rapid Resolution Liquid Chromatography/Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jian-Fei Qin

    2013-09-01

    Full Text Available A rapid resolution liquid chromatography/time-of-flight tandem mass spectrometry (RRLC-TOF/MS method was developed for qualitative and quantitative analysis of the major chemical constituents in Andrographis paniculata. Fifteen compounds, including flavonoids and diterpenoid lactones, were unambiguously or tentatively identified in 10 min by comparing their retention times and accurate masses with standards or literature data. The characteristic fragmentation patterns of flavonoids and diterpenoid lactones were summarized, and the structures of the unknown compounds were predicted. Andrographolide, dehydroandrographolide and neoandrographolide were further quantified as marker substances. It was found that the calibration curves for all analytes showed good linearity (R2 > 0.9995 within the test ranges. The overall limits of detection (LODs and limits of quantification (LOQs were 0.02 μg/mL to 0.06 μg/mL and 0.06 μg/mL to 0.2 μg/mL, respectively. The relative standard deviations (RSDs for intra- and inter-day precisions were below 3.3% and 4.2%, respectively. The mean recovery rates ranged from 96.7% to 104.5% with the relative standard deviations (RSDs less than 2.72%. It is concluded that RRLC-TOF/MS is powerful and practical in qualitative and quantitative analysis of complex plant samples due to time savings, sensitivity, precision, accuracy and lowering solvent consumption.

  15. A combined segmented anode gas ionization chamber and time-of-flight detector for heavy ion elastic recoil detection analysis

    Science.gov (United States)

    Ström, Petter; Petersson, Per; Rubel, Marek; Possnert, Göran

    2016-10-01

    A dedicated detector system for heavy ion elastic recoil detection analysis at the Tandem Laboratory of Uppsala University is presented. Benefits of combining a time-of-flight measurement with a segmented anode gas ionization chamber are demonstrated. The capability of ion species identification is improved with the present system, compared to that obtained when using a single solid state silicon detector for the full ion energy signal. The system enables separation of light elements, up to Neon, based on atomic number while signals from heavy elements such as molybdenum and tungsten are separated based on mass, to a sample depth on the order of 1 μm. The performance of the system is discussed and a selection of material analysis applications is given. Plasma-facing materials from fusion experiments, in particular metal mirrors, are used as a main example for the discussion. Marker experiments using nitrogen-15 or oxygen-18 are specific cases for which the described improved species separation and sensitivity are required. Resilience to radiation damage and significantly improved energy resolution for heavy elements at low energies are additional benefits of the gas ionization chamber over a solid state detector based system.

  16. Laser desorption/ionization time-of-flight mass spectrometry of triacylglycerols and other components in fingermark samples.

    Science.gov (United States)

    Emerson, Beth; Gidden, Jennifer; Lay, Jackson O; Durham, Bill

    2011-03-01

    The chemical composition of fingermarks could potentially be important for determining investigative leads, placing individuals at the time of a crime, and has applications as biomarkers of disease. Fingermark samples containing triacylglycerols (TAGs) and other components were analyzed using laser desorption/ionization (LDI) time-of-flight mass spectrometry (TOF MS). Only LDI appeared to be useful for this application while conventional matrix-assisted LDI-TOF MS was not. Tandem MS was used to identify/confirm selected TAGs. A limited gender comparison, based on a simple t-distribution and peaks intensities, indicated that two TAGs showed gender specificity at the 95% confidence level and two others at 97.5% confidence. Because gender-related TAGs differences were most often close to the standard deviation of the measurements, the majority of the TAGs showed no gender specificity. Thus, LDI-TOF MS is not a reliable indicator of gender based on fingermark analysis. Cosmetic ingredients present in some samples were identified. © 2011 American Academy of Forensic Sciences.

  17. Profiling analysis of low molecular weight heparins by multiple heart-cutting two dimensional chromatography with quadruple time-of-flight mass spectrometry.

    Science.gov (United States)

    Ouyang, Yilan; Zeng, Yangyang; Rong, Yinxiu; Song, Yue; Shi, Lv; Chen, Bo; Yang, Xinlei; Xu, Naiyu; Linhardt, Robert J; Zhang, Zhenqing

    2015-09-01

    Low molecular weight heparins (LMWHs) are polydisperse and microheterogenous mixtures of polysaccharides used as anticoagulant drugs. Profiling analysis is important for obtaining deeper insights into the structure of LMWHs. Previous oligosaccharide mapping methods are relatively low resolution and are unable to show an entire picture of the structural complexity of LMWHs. In the current study a profiling method was developed relying on multiple heart-cutting, two-dimensional, ultrahigh performance liquid chromatography with quadruple time-of-flight mass spectrometry. This represents an efficient, automated, and robust approach for profiling LMWHs. Using size-exclusion chromatography and ion-pairing reversed-phase chromatography in a two-dimensional separation, LMW components of different sizes and LMW components of the same size but with different charges and polarities can be resolved, providing a more complete picture of a LMWH. Structural information on each component was then obtained with quadrupole time-of-flight mass spectrometry. More than 80 and 120 oligosaccharides were observed and unambiguously assigned from the LMWHs, nadroparin and enoxaparin, respectively. This method might be useful for quality control of LMWHs and as a powerful tool for heparin-related glycomics.

  18. Development and validation of a simple solid-phase extraction method coupled with liquid chromatography-triple quadrupole tandem mass spectrometry for simultaneous determination of lincomycin, tylosin A and tylosin B in royal jelly.

    Science.gov (United States)

    Zheng, Weijia; Park, Jin-A; Abd El-Aty, A M; Kim, Seong-Kwan; Cho, Sang-Hyun; Choi, Jeong-Min; Warda, Mohamad; Wang, Jing; Shim, Jae-Han; Shin, Ho-Chul

    2018-04-01

    We have developed an analytical method for the determination of lincomycin, tylosin A and tylosin B residues in royal jelly using liquid chromatography-triple quadrupole tandem mass spectrometry analysis. For extraction and purification, we employed 1% trifluoroacetic acid and 0.1 m Na 2 EDTA solutions along with an Oasis HLB cartridge. The target antibiotics were well separated in a Kinetex EVO C 18 reversed-phase analytical column using a combination of 0.1% formate acid in ultrapure water (A) and acetonitrile (B) as the mobile phase. Good linearity was achieved over the tested concentration range (5-50 μg/kg) in matrix-matched standard calibration. The coefficients of determination (R 2 ) were 0.9933, 0.9933 and 0.996, for tylosin A, tylosin B and lincomycin, respectively. Fortified royal jelly spiked with three different concentrations of the tested antibiotics (5, 10 and 20 μg/kg) yielded recoveries in the range 80.94-109.26% with relative standard deviations ≤4%. The proposed method was applied to monitor 11 brand of royal jelly collected from domestic markets and an imported brand from New Zealand; all the samples tested negative for lincomycin, tylosin A and tylosin B residues. In conclusion, 1% trifluoroacetic acid and 0.1 m Na 2 EDTA aqueous solvents combined with solid-phase extraction could effectively complete the sample preparation process for royal jelly before analysis. The developed approach can be applied for a routine analysis of lincomycin, tylosin A and tylosin B residues in royal jelly. Copyright © 2017 John Wiley & Sons, Ltd.

  19. Comparative analysis of main bio-active components in the herb pair Danshen-Honghua and its single herbs by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Qu, Cheng; Pu, Zong-Jin; Zhou, Gui-Sheng; Wang, Jun; Zhu, Zhen-Hua; Yue, Shi-Jun; Li, Jian-Ping; Shang, Li-Li; Tang, Yu-Ping; Shi, Xu-Qin; Liu, Pei; Guo, Jian-Ming; Sun, Jing; Tang, Zhi-Shu; Zhao, Jing; Zhao, Bu-Chang; Duan, Jin-Ao

    2017-09-01

    A sensitive, reliable, and powerful ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry method was developed for simultaneous quantification of the 15 main bio-active components including phenolic acids and flavonoids within 13 min for the first time. The proposed method was first reported and validated by good linearity (r 2  > 0.9975), limit of detection (1.12-7.01 ng/mL), limit of quantification (3.73-23.37 ng/mL), intra- and inter-day precisions (RSD ≤ 1.92%, RSD ≤ 2.45%), stability (RSD ≤ 5.63%), repeatability (RSD ≤ 4.34%), recovery (96.84-102.12%), and matrix effects (0.92-1.02). The established analytical methodology was successfully applied to comparative analysis of main bio-active components in the herb pair Danshen-Honghua and its single herbs. Compared to the single herb, the content of most flavonoid glycosides was remarkably increased in their herb pair, and main phenolic acids were decreased, conversely. The content changes of the main components in the herb pair supported the synergistic effects on promoting blood circulation and removing blood stasis. The results provide a scientific basis and reference for the quality control of Danshen-Honghua herb pair and the drug interactions based on variation of bio-active components in herb pairs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Potential of gas chromatography-orthogonal acceleration time-of-flight mass spectrometry (GC-oaTOFMS) in flavor research.

    Science.gov (United States)

    Fay, Laurent B; Newton, Anthony; Simian, Hervé; Robert, Fabien; Douce, David; Hancock, Peter; Green, Martin; Blank, Imre

    2003-04-23

    Gas chromatography-orthogonal acceleration time-of-flight mass spectrometry (GC-oaTOFMS) is an emerging technique offering a straightforward access to a resolving power up to 7000. This paper deals with the use of GC-oaTOFMS to identify the flavor components of a complex seafood flavor extract and to quantify furanones formed in model Maillard reactions. A seafood extract was selected as a representative example for complex food flavors and was previously analyzed using GC-quadrupole MS, leaving several molecules unidentified. GC-oaTOFMS analysis was focused on these unknowns to evaluate its potential in flavor research, particularly for determining exact masses. N-Methyldithiodimethylamine, 6-methyl-5-hepten-2-one, and tetrahydro-2,4-dimethyl-4H-pyrrolo[2,1-d]-1,3,5-dithiazine were successfully identified on the basis of the precise mass determination of their molecular ions and their major fragments. A second set of experiments was performed to test the capabilities of the GC-oaTOFMS for quantification. Calibration curves were found to be linear over a dynamic range of 10(3) for the quantification of furanones. The quantitative data obtained using GC-oaTOFMS confirmed earlier results that the formation of 4-hydroxy-2,5-dimethyl-3(2H)-furanone was favored in the xylose/glycine model reaction and 2(or 5)-ethyl-4-hydroxy-5(or 2)-methyl-3(2H)-furanone in the xylose/alanine model reaction. It was concluded that GC-oaTOFMS may become a powerful analytical tool for the flavor chemist for both identification and quantification purposes, the latter in particular when combined with stable isotope dilution assay.

  1. Comparison of linear intrascan and interscan dynamic ranges of Orbitrap and ion-mobility time-of-flight mass spectrometers.

    Science.gov (United States)

    Kaufmann, Anton; Walker, Stephan

    2017-11-30

    The linear intrascan and interscan dynamic ranges of mass spectrometers are important in metabolome and residue analysis. A large linear dynamic range is mandatory if both low- and high-abundance ions have to be detected and quantitated in heavy matrix samples. These performance criteria, as provided by modern high-resolution mass spectrometry (HRMS), were systematically investigated. The comparison included two generations of Orbitraps, and an ion mobility quadrupole time-of-flight (QTOF) system In addition, different scan modes, as provided by the utilized instruments, were investigated. Calibration curves of different compounds covering a concentration range of five orders of magnitude were measured to evaluate the linear interscan dynamic range. The linear intrascan dynamic range and the resulting mass accuracy were evaluated by repeating these measurements in the presence of a very intense background. Modern HRMS instruments can show linear dynamic ranges of five orders of magnitude. Often, however, the linear dynamic range is limited by the detection capability (sensitivity and selectivity) and by the electrospray ionization. Orbitraps, as opposed to TOF instruments, show a reduced intrascan dynamic range. This is due to the limited C-trap and Orbitrap capacity. The tested TOF instrument shows poorer mass accuracies than the Orbitraps. In contrast, hyphenation with an ion-mobility device seems not to affect the linear dynamic range. The linear dynamic range of modern HRMS instrumentation has been significantly improved. This also refers to the virtual absence of systematic mass shifts at high ion abundances. The intrascan dynamic range of the current Orbitrap technology may still be a limitation when analyzing complex matrix extracts. On the other hand, the linear dynamic range is not only limited by the detector technology, but can also be shortened by peripheral devices, where the ionization and transfer of ions take place. Copyright © 2017 John Wiley

  2. Monte-Carlo studies of the performance of scintillator detectors for time-of-flight measurements

    International Nuclear Information System (INIS)

    Yang, X.H.

    1995-01-01

    In this paper we report on a Monte-Carlo program, SToF, developed to evaluate the performance of scintillator-based Time-of-Flight (TOF) detectors. This program has been used in the design of the TOF system for the PHENIX experiment at RHIC. The program was used to evaluate the intrinsic time-of-flight resolution of various scintillator and light-guide geometries, and the results of these simulations are presented here. The simulation results agree extremely well with measured pulse-height and time distributions with one adjustable parameter. These results, thus, explain also the reduced quantities, such as the position dependence of the time resolution, etc, implying that SToF will be generally useful for estimating the performance of TOF detectors. ((orig.))

  3. Time of flight and range of the motion of a projectile in a constant gravitational field

    Directory of Open Access Journals (Sweden)

    P. A. Karkantzakos

    2009-01-01

    Full Text Available In this paper we study the classical problem of the motion of a projectile in a constant gravitational field under the influenceof a retarding force proportional to the velocity. Specifically, we express the time of flight, the time of fall and the range ofthe motion as a function of the constant of resistance per unit mass of the projectile. We also prove that the time of fall isgreater than the time of rise with the exception of the case of zero constant of resistance where we have equality. Finally weprove a formula from which we can compute the constant of resistance per unit mass of the projectile from time of flight andrange of the motion when the acceleration due to gravity and the initial velocity of the projectile are known.

  4. Neutron Time-of-Flight Quantification of Water Desorption Isotherms of Montmorillonite

    DEFF Research Database (Denmark)

    Gates, Will P.; Bordallo, Heloisa N.; Aldridge, Laurence P.

    2012-01-01

    enabled us to differentiate at least two water motions during dehydration of Ca- and Na-SAz-1 (initially equilibrated at RH = 55%) by using a "controlled water loss" time-of-flight procedure. This work confirms that (a) interlayer and cationic water in dioctahedral smectites are characterized by slower...... motions than interparticle water, (b) interlayer cations influenced the dynamics of water loss, probably through its affect on clay fabric, and (c) interparticle water behaves more like bulk water. At 55% RH the Ca montmorillonite held more interparticle water, but on dehydration under controlled......The multiple energy states of water held by surfaces of a clay mineral can be effectively probed with time-of-flight and fixed elastic window neutron scattering. We used these techniques to quantitatively differentiate water types, including rotational and translational diffusions, in Ca- and Na...

  5. Particle identification by time-of-flight measurement in the SAPHIR

    International Nuclear Information System (INIS)

    Hoffmann-Rothe, P.

    1993-02-01

    Using photoproduction data which have been measured with the SAPHIR-detector with different target materials (C H 2 solid , H 2 liquid , D 2 liquid ) a detailed investigation and discussion of the detectors performance to measure the time of flight of charged particles and to separate between particles of different mass has been accomplished. A FORTRAN program has been written which provides a calibration of the scintillator panels of the TOF hodoscopes, calculates correction factors for the time-walk effect an finally, by combining the time of flight with track momentum measurement, determines particle masses. The current configuration of the detector makes it possible to separate between proton and pion up to a particle momentum of 1.6 GeV/c. Proton and kaon can be separated up to a momentum of 1.3 GeV/c, kaon and pion up to a momentum of 0.85 GeV/c. (prog.) [de

  6. The time-of-flight TOFW detector of the HARP experiment: construction and performance

    International Nuclear Information System (INIS)

    Baldo-Ceolin, M.; Barichello, G.; Bobisut, F.; Bonesini, M.; De Min, A.; Ferri, A.F.; Gibin, D.; Guglielmi, A.; Laveder, M.; Menegolli, A.; Mezzetto, M.; Paganoni, M.; Paleari, F.; Pepato, A.; Tonazzo, A.; Vascon, M.

    2004-01-01

    The construction and performance of a large area scintillator-based time-of-flight detector for the HARP experiment at CERN are reported. An intrinsic counter time resolution of ∼160 ps was achieved. The precision on the time calibration and monitoring of the detector was maintained at better than 100 ps by using dedicated cosmic rays runs, a fast laser-based system and calibrations with beam particles. The detector was operated on the T9 PS beamline during 2001 and 2002. A time-of-flight resolution of ∼200 ps was obtained, providing π/p discrimination at more than 3σ up to 4.0 GeV/c momentum

  7. The Dubna double-arm time-of-flight spectrometer for heavy-ion reaction products

    International Nuclear Information System (INIS)

    Schilling, K.D.; Gippner, P.; Seidel, W.; Stary, F.; Will, E.; Heidel, K.; Lukyanov, S.M.; Penionzhkevich, Yu.E.; Salamatin, V.S.; Sodan, H.; Chubarian, G.G.

    1986-05-01

    The double-arm time-of-flight spectrometer DEMAS designed for the detection and identification of heavy-ion reaction products at incident energies below 10 MeV/amu is presented. Based on the kinematic coincidence method, the relevant physical information is obtained from the measurement of the two correlated velocity vectors of the binary fragments. Construction and performance of the different detector systems applied to measure the time-of-flight values, the position coordinates and the kinetic energies of both fragments are presented in detail. The description of the data acquisition and analysing procedures is followed by the discussion of some experimental examples to demonstrate the spectrometer performance. A mass resolution of typically 4 - 5 amu (fwhm) is routinely achieved. (author)

  8. Time-of-flight spectrometer for the measurement of gamma correlated neutron spectra

    International Nuclear Information System (INIS)

    Andriashin, A.V.; Devkin, B.V.; Lychagin, A.A.; Minko, J.V.; Mironov, A.N.; Nesterenko, V.S.; Sztaricskai, T.; Petoe, G.; Vasvary, L.

    1986-01-01

    A time-of-flight spectrometer for the measurement of gamma correlated neutron spectra from (n,xnγ) reactions is described. The operation and the main parameters are discussed. The resolution in the neutron channel is 2.2 ns/m at the 150 keV neutron energy threshold. A simultaneous measurement of the time-of-flight and amplitude distributions makes it possible to study gamma correlated neutron spectra as well as the prompt gamma spectra in coincidence with selected energy neutrons. In order to test the spectrometer, measurements of the neutron spectrum in coincidence with the 846 keV gamma line of 56 Fe were carried out at an incident neutron energy of 14.1 MeV. (Auth.)

  9. Time-of-flight spectrometer for the measurement of gamma correlated neutron spectra

    International Nuclear Information System (INIS)

    Andryashin, A.V.; Devlein, B.V.; Lychagin, A.A.; Minko, Y.V.; Mironov, A.N.; Nesterenko, V.S.

    1986-01-01

    A time-of-flight spectrometer for the measurement of gamma correlated neutron spectra form (n,xnγ) reactions is described. The operation and the main parameters are discussed. The resolution in the neutron channel is 2.2 ns/m at the 150 keV neutron energy threshold. A simultaneous measurement of the time-of-flight and amplitude distributions makes it possible to study gamma correlated neutron spectra as well as the prompt gamma spectra in coincidence with selected energy neutrons. In order to test the spectrometer, measurements of the neutron spectrum in coincidence with the 846 keV gamma line of 56 Fe were carried out at an incident neutron energy of 14.1 MeV. (author). 3 figs., 6 refs

  10. A new method of detection for a positron emission tomograph using a time of flight method

    International Nuclear Information System (INIS)

    Gresset, Christian.

    1981-05-01

    In the first chapter, it is shown the advantages of positron radioemitters (β + ) of low period, and the essential characteristics of positron tomographs realized at the present time. The second chapter presents the interest of an original technique of image reconstruction: the time of flight technique. The third chapter describes the characterization methods which were set for verifying the feasibility of cesium fluoride in tomography. Chapter four presents the results obtained by these methods. It appears that the cesium fluoride constitute presently the best positron emission associated to time of flight technique. The hypotheses made on eventual performances of such machines are validated by experiments with phantom. The results obtained with a detector (bismuth germanate) conserves all its interest in skull tomography [fr

  11. Beam derived trigger system for multibunch time-of-flight measurement

    International Nuclear Information System (INIS)

    Fox, J.; Pellegrin, J.L.

    1981-01-01

    Particle time-of-flight measurement requires accurate triggers in synchronism with each bunch, and occurring in a sequence which depends on the position of the observer around the storage ring. A system has been devised for tagging the colliding bunches at each interaction point; it allows one to record which pair of bunches is colliding at any time and any location around the machine. Besides bunch identification, the time-of-flight triggers are also expected to have a time stability better than the bunch length itself. A system is presented here which exhibits time variations of less than 80 psec over a 20 to 1 range of beam current, while the jitter is at least an order of magnitude smaller. 4 refs., 4 figs

  12. Time of flight measurements of unirradiated and irradiated nuclear graphite under cyclic compressive load

    Energy Technology Data Exchange (ETDEWEB)

    Bodel, W., E-mail: william.bodel@hotmail.com [Nuclear Graphite Research Group, The University of Manchester (United Kingdom); Atkin, C. [Health and Safety Laboratory, Buxton (United Kingdom); Marsden, B.J. [Nuclear Graphite Research Group, The University of Manchester (United Kingdom)

    2017-04-15

    The time-of-flight technique has been used to investigate the stiffness of nuclear graphite with respect to the grade and grain direction. A loading rig was developed to collect time-of-flight measurements during cycled compressive loading up to 80% of the material's compressive strength and subsequent unloading of specimens along the axis of the applied stress. The transmission velocity (related to Young's modulus), decreased with increasing applied stress; and depending on the graphite grade and orientation, the modulus then increased, decreased or remained constant upon unloading. These tests were repeated while observing the microstructure during the load/unload cycles. Initial decreases in transmission velocity with compressive load are attributed to microcrack formation within filler and binder phases. Three distinct types of behaviour occur on unloading, depending on the grade, irradiation, and loading direction. These different behaviours can be explained in terms of the material microstructure observed from the microscopy performed during loading.

  13. A compact time-of-flight mass spectrometer for ion source characterization

    International Nuclear Information System (INIS)

    Chen, L.; Wan, X.; Jin, D. Z.; Tan, X. H.; Huang, Z. X.; Tan, G. B.

    2015-01-01

    A compact time-of-flight mass spectrometer with overall dimension of about 413 × 250 × 414 mm based on orthogonal injection and angle reflection has been developed for ion source characterization. Configuration and principle of the time-of-flight mass spectrometer are introduced in this paper. The mass resolution is optimized to be about 1690 (FWHM), and the ion energy detection range is tested to be between about 3 and 163 eV with the help of electron impact ion source. High mass resolution and compact configuration make this spectrometer useful to provide a valuable diagnostic for ion spectra fundamental research and study the mass to charge composition of plasma with wide range of parameters

  14. Measurement and simulation of the inelastic resolution function of a time-of-flight spectrometer

    International Nuclear Information System (INIS)

    Roth, S.V.; Zirkel, A.; Neuhaus, J.; Petry, W.; Bossy, J.; Peters, J.; Schober, H.

    2002-01-01

    The deconvolution of inelastic neutron scattering data requires the knowledge of the inelastic resolution function. The inelastic resolution function of the time-of-flight spectrometer IN5/ILL has been measured by exploiting the sharp resonances of the roton and maxon excitations in superfluid 4 He for the two respective (q,ω) values. The calculated inelastic resolution function for three different instrumental setups is compared to the experimentally determined resolution function. The agreement between simulation and experimental data is excellent, allowing us in principle to extrapolate the simulations and thus to determine the resolution function in the whole accessible dynamic range of IN5 or any other time-of-flight spectrometer. (orig.)

  15. Measurement and simulation of the inelastic resolution function of a time-of-flight spectrometer

    CERN Document Server

    Roth, S V; Neuhaus, J; Petry, W; Bossy, J; Peters, J; Schober, H

    2002-01-01

    The deconvolution of inelastic neutron scattering data requires the knowledge of the inelastic resolution function. The inelastic resolution function of the time-of-flight spectrometer IN5/ILL has been measured by exploiting the sharp resonances of the roton and maxon excitations in superfluid sup 4 He for the two respective (q,omega) values. The calculated inelastic resolution function for three different instrumental setups is compared to the experimentally determined resolution function. The agreement between simulation and experimental data is excellent, allowing us in principle to extrapolate the simulations and thus to determine the resolution function in the whole accessible dynamic range of IN5 or any other time-of-flight spectrometer. (orig.)

  16. Cross-correlation time-of-flight analysis of molecular beam scattering

    International Nuclear Information System (INIS)

    Nowikow, C.V.; Grice, R.

    1979-01-01

    The theory of the cross-correlation method of time-of-flight analysis is presented in a form which highlights its formal similarity to the conventional method. A time-of-flight system for the analysis of crossed molecular beam scattering is described, which is based on a minicomputer interface and can operate in both the cross-correlation and conventional modes. The interface maintains the synchronisation of chopper disc rotation and channel advance indefinitely in the cross-correlation method and can acquire data in phase with the beam modulation in both methods. The shutter function of the cross-correlation method is determined and the deconvolution analysis of the data is discussed. (author)

  17. Digitizing data acquisition and time-of-flight pulse processing for ToF-ERDA

    Energy Technology Data Exchange (ETDEWEB)

    Julin, Jaakko, E-mail: jaakko.julin@jyu.fi; Sajavaara, Timo

    2016-01-01

    A versatile system to capture and analyze signals from multi channel plate (MCP) based time-of-flight detectors and ionization based energy detectors such as silicon diodes and gas ionization chambers (GIC) is introduced. The system is based on commercial digitizers and custom software. It forms a part of a ToF-ERDA spectrometer, which has to be able to detect recoil atoms of many different species and energies. Compared to the currently used analogue electronics the digitizing system provides comparable time-of-flight resolution and improved hydrogen detection efficiency, while allowing the operation of the spectrometer be studied and optimized after the measurement. The hardware, data acquisition software and digital pulse processing algorithms to suit this application are described in detail.

  18. Invited Article: Characterization of background sources in space-based time-of-flight mass spectrometers

    International Nuclear Information System (INIS)

    Gilbert, J. A.; Gershman, D. J.; Gloeckler, G.; Lundgren, R. A.; Zurbuchen, T. H.; Orlando, T. M.; McLain, J.; Steiger, R. von

    2014-01-01

    For instruments that use time-of-flight techniques to measure space plasma, there are common sources of background signals that evidence themselves in the data. The background from these sources may increase the complexity of data analysis and reduce the signal-to-noise response of the instrument, thereby diminishing the science value or usefulness of the data. This paper reviews several sources of background commonly found in time-of-flight mass spectrometers and illustrates their effect in actual data using examples from ACE-SWICS and MESSENGER-FIPS. Sources include penetrating particles and radiation, UV photons, energy straggling and angular scattering, electron stimulated desorption of ions, ion-induced electron emission, accidental coincidence events, and noise signatures from instrument electronics. Data signatures of these sources are shown, as well as mitigation strategies and design considerations for future instruments

  19. Dual cascade time-of-flight mass spectrometer basing on electrostatic mirrors with two dimensional fields

    International Nuclear Information System (INIS)

    Glikman, L. G.; Goloskokov, Yu. V.; Karetskaya, S.P.; Mit', A.G.

    1999-01-01

    In the report [1] we have suggested the scheme of time-of-flight spectrometer containing two electrostatic mirrors with two dimensional field that doesn't depend on one of the Cartesian coordinates). In the articles [2,3] there have been found conditions for obtaining high quality of time-of-flight and spatial focusing. One of basic advantages of this scheme - is availability of intermediate stigmatic image. In the plane where this image is it's possible to place controlled diaphragm that limits ion scatter along the energy if the scatter is too large. With the help of this diaphragm at the spectrometer you can register mass spectrum with the selected energy. Good focusing quality allows reducing of initial ion energy by this increasing the time of their flight and thus analyzers resolving ability. Ion source and receiver are spaced at rather a long distances. This can be useful to solve some practical tasks

  20. Rietveld refinement with time-of-flight powder diffraction data from pulsed neutron sources

    International Nuclear Information System (INIS)

    David, W.I.F.; Jorgensen, J.D.

    1990-10-01

    The recent development of accelerator-based pulsed neutron sources has led to the widespread use of the time-of-flight technique for neutron powder diffraction. The properties of the pulsed source make possible unusually high resolution over a wide range of d spacings, high count rates, and the ability to collect complete data at fixed scattering angles. The peak shape and other instrument characteristics can be accurately modelled, which make Rietveld refinement possible for complex structures. In this paper we briefly review the development of the Rietveld method for time-of-flight diffraction data from pulsed neutron sources and discuss the latest developments in high resolution instrumentation and advanced Rietveld analysis methods. 50 refs., 12 figs., 14 tabs

  1. Computational imaging with multi-camera time-of-flight systems

    KAUST Repository

    Shrestha, Shikhar

    2016-07-11

    Depth cameras are a ubiquitous technology used in a wide range of applications, including robotic and machine vision, human computer interaction, autonomous vehicles as well as augmented and virtual reality. In this paper, we explore the design and applications of phased multi-camera time-of-flight (ToF) systems. We develop a reproducible hardware system that allows for the exposure times and waveforms of up to three cameras to be synchronized. Using this system, we analyze waveform interference between multiple light sources in ToF applications and propose simple solutions to this problem. Building on the concept of orthogonal frequency design, we demonstrate state-of-the-art results for instantaneous radial velocity capture via Doppler time-of-flight imaging and we explore new directions for optically probing global illumination, for example by de-scattering dynamic scenes and by non-line-of-sight motion detection via frequency gating. © 2016 ACM.

  2. Measurement of fast assembly spectra using time-of-flight method

    International Nuclear Information System (INIS)

    Duquesne, Henry; Rotival, Michel; Schmitt, Andre; Allard, Christian; De Keyser, Albert; Hortsmann, Henri

    1975-07-01

    Measurement of neutron spectra made in fast subcritical assemblies HUG 3 and PHUG 3 (uranium-graphite and plutonium-graphite) utilizing time-of-flight techniques are described. The matrix were excited by the pulsed neutron source from the BCMN Linac beam impinging on a target of natural uranium. Details of the experimental procedure, safety studies, detector calibration and data reduction are given [fr

  3. Time-of-flight and vector polarization analysis for diffuse neutron scattering

    International Nuclear Information System (INIS)

    Schweika, W.

    2003-01-01

    The potential of pulsed neutron sources for diffuse scattering including time-of-flight (TOF) and polarization analysis is discussed in comparison to the capabilities of the present instrument diffuse neutron scattering at the research center Juelich. We present first results of a new method for full polarization analysis using precessing neutron polarization. A proposal is made for a new type of instrument at pulsed sources, which allows for vector polarization analysis in TOF instruments with multi-detectors

  4. Parameters’ Covariance in Neutron Time of Flight Analysis – Explicit Formulae

    Energy Technology Data Exchange (ETDEWEB)

    Odyniec, M. [NSTec; Blair, J. [NSTec

    2014-12-01

    We present here a method that estimates the parameters’ variance in a parametric model for neutron time of flight (NToF). The analytical formulae for parameter variances, obtained independently of calculation of parameter values from measured data, express the variances in terms of the choice, settings, and placement of the detector and the oscilloscope. Consequently, the method can serve as a tool in planning a measurement setup.

  5. Influence of absorption on the time of flight of the light going through a complex medium

    Directory of Open Access Journals (Sweden)

    M. Kervella

    2011-09-01

    Full Text Available The aim of this work is to evaluate the influence of absorption processes on the time of flight of light going through an absorbing and scattering thick medium (clouds, paints, gas cell, etc. In order to study statistical scattering and absorbing processes, we use a Monte-Carlo simulation code with temporal phase function and Debye modes. The main result is that absorption inside particles induces a decrease of the global time delay.

  6. History and current status of PET development based on time of flight

    International Nuclear Information System (INIS)

    Yun Mingkai; Li Ting; Zhang Zhiming; Zhang Yubao; Shan Baoci; Wei Long

    2012-01-01

    The principle of time of flight (TOF) positron emission tomography (PET) and a brief review of the history of TOF-PET are introduced. The factors influencing the time resolution of a TOF-PET scanner are presented, especially focus on the intrinsic properties of scintillators and front-end electronics. Challenges and achievements of the structure of data organization and image reconstruction are reviewed. Finally, the benefits of TOF-PET on image quality improvement and tumor detection are emphasized. (authors)

  7. Identification of microorganisms using superconducting tunnel junctions and time-of-flight mass spectrometry

    Science.gov (United States)

    Ullom, J. N.; Frank, M.; Horn, J. M.; Labov, S. E.; Langry, K.; Benner, W. H.

    2000-04-01

    We present time-of-flight measurements of biological material ejected from bacterial spores following laser irradiation. Ion impacts are registered on a microchannel plate detector and on a Superconducting Tunnel Junction (STJ) detector. We compare mass spectra obtained with the two detectors. The STJ has better sensitivity to massive ions and also measures the energy of each ion. We show evidence that spores of different bacillus species produce distinctive mass spectra and associate the observed mass peaks with coat proteins.

  8. Identification of microorganisms using superconducting tunnel junctions and time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Ullom, J.N.; Frank, M.; Horn, J.M.; Labov, S.E.; Langry, K.; Benner, W.H.

    2000-01-01

    We present time-of-flight measurements of biological material ejected from bacterial spores following laser irradiation. Ion impacts are registered on a microchannel plate detector and on a Superconducting Tunnel Junction (STJ) detector. We compare mass spectra obtained with the two detectors. The STJ has better sensitivity to massive ions and also measures the energy of each ion. We show evidence that spores of different bacillus species produce distinctive mass spectra and associate the observed mass peaks with coat proteins

  9. Neutron xyz - polarization analysis at a time-of-flight instrument

    Energy Technology Data Exchange (ETDEWEB)

    Ehlers, Georg [ORNL; Stewart, John Ross [ISIS Facility, Rutherford Appleton Laboratory; Andersen, Ken [ESS

    2015-01-01

    When implementing a dedicated polarization analysis setup at a neutron time-of-flight instrument with a large area detector, one faces enormous challenges. Nevertheless, significant progress has been made towards this goal over the last few years. This paper addresses systematic limitations of the traditional method that is used to make these measurements, and a possible strategy to overcome these limitations. This will be important, for diffraction as well as inelastic experiments, where the scattering occurs mostly out-of-plane.

  10. Testing the time-of-flight model for flagellar length sensing.

    Science.gov (United States)

    Ishikawa, Hiroaki; Marshall, Wallace F

    2017-11-07

    Cilia and flagella are microtubule-based organelles that protrude from the surface of most cells, are important to the sensing of extracellular signals, and make a driving force for fluid flow. Maintenance of flagellar length requires an active transport process known as intraflagellar transport (IFT). Recent studies reveal that the amount of IFT injection negatively correlates with the length of flagella. These observations suggest that a length-dependent feedback regulates IFT. However, it is unknown how cells recognize the length of flagella and control IFT. Several theoretical models try to explain this feedback system. We focused on one of the models, the "time-of-flight" model, which measures the length of flagella on the basis of the travel time of IFT protein in the flagellar compartment. We tested the time-of-flight model using Chlamydomonas dynein mutant cells, which show slower retrograde transport speed. The amount of IFT injection in dynein mutant cells was higher than that in control cells. This observation does not support the prediction of the time-of-flight model and suggests that Chlamydomonas uses another length-control feedback system rather than that described by the time-of-flight model. © 2017 Ishikawa and Marshall. This article is distributed by The American Society for Cell Biology under license from the author(s). Two months after publication it is available to the public under an Attribution–Noncommercial–Share Alike 3.0 Unported Creative Commons License (http://creativecommons.org/licenses/by-nc-sa/3.0).

  11. Time-of-flight studies of multiple Bragg reflections in cylindrically bent perfect crystals

    Czech Academy of Sciences Publication Activity Database

    Mikula, Pavol; Furusaka, M.; Ohkubob, K.; Šaroun, Jan

    2012-01-01

    Roč. 45, č. 12 (2012), s. 1248-1253 ISSN 0021-8898 R&D Projects: GA AV ČR KJB100480901; GA ČR GAP204/10/0654 Institutional support: RVO:61389005 Keywords : neutron diffraction * time-of-flight method * multiple reflections * bent perfect crystals Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 3.343, year: 2012

  12. Development of a hand-portable photoionization time-of-flight mass spectrometer

    International Nuclear Information System (INIS)

    Dieckman, S.L.; Bostrom, G.A.; Waterfield, L.G.; Jendrzejczyk, J.A.; Raptis, A.C.

    1996-01-01

    ANL is currently developing a portable chemical sensor system based on laser desorption photoionization time-of-flight mass spectrometry. It will incorporate direct sampling, a cryocooler base sample adsorption and concentration, and direct surface multiphoton ionization. All components will be in a package 9 x 11 x 4 in., weighing 15-18 lbs. A sample spectrum is given for a NaCl sample

  13. The advantages of orthogonal acceleration in ICP time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Gaal, Andrew

    2004-01-01

    The OptiMass 8000 incorporates an orthogonal acceleration time-of-flight mass spectrometer. A general schematic of the instrument is given. The continuous ion beam is chopped by an orthogonal accelerator. A push out pulse supply is coupled to the accelerator for providing repetitive push-out voltages at a frequency of 30 kHz. The ion packets that are sliced out of the beam then travel within the field free space towards the SMARTGATE ion blanker. Orthogonal accelerator parameters are set to enable temporal-spatial focusing at the SMARTGATE ion blanker, so that iso-mass ion packets are resolved in time. Any ion packets of unwanted specie are ejected from the direction of travel by supplying pulsed voltages onto the deflection plates of the SMARTGATE. The ions to be measured are let through SMARTGATE and travel further down the field free space, to enter the ion reflectron. The ion reflectron increases the resolution of the mass spectrometer by means of temporal-energy focussing. After reflection, the ions travel within the field free space towards the discrete-dynode detector. In comparison to other acceleration geometries used in elemental time-of-flight mass spectrometry the OptiMass 8000 orthogonal acceleration geometry ultimately leads to superior resolution. As the energy spread is about 3 orders of magnitude lower in the time-of-flight direction for an oaTOFMS in comparison to an on-axis system, aberration acquired in the initial stages of acceleration are much lower. As a result the orthogonal acceleration scheme provides superior resolution at the first spatial focus point and the detector. The orthogonal acceleration time-of-flight analyzer of the OptiMass 8000 is able to provide resolution of at least 1800 at mass 238. (author)

  14. Timing performances of a data acquisition system for Time of Flight PET

    International Nuclear Information System (INIS)

    Morrocchi, Matteo; Marcatili, Sara; Belcari, Nicola; Bisogni, Maria G.; Collazuol, Gianmaria; Ambrosi, Giovanni; Corsi, Francesco; Foresta, Maurizio; Marzocca, Cristoforo; Matarrese, Gianvito; Sportelli, Giancarlo; Guerra, Pedro; Santos, Andres; Del Guerra, Alberto

    2012-01-01

    We are investigating the performances of a data acquisition system for Time of Flight PET, based on LYSO crystal slabs and 64 channels Silicon Photomultipliers matrices (1.2 cm 2 of active area each). Measurements have been performed to test the timing capability of the detection system (SiPM matices coupled to a LYSO slab and the read-out electronics) with both test signal and radioactive source.

  15. Timing performances of a data acquisition system for Time of Flight PET

    Energy Technology Data Exchange (ETDEWEB)

    Morrocchi, Matteo, E-mail: matteo.morrocchi@pi.infn.it [University of Pisa and INFN Sezione di Pisa, I 56127 Pisa (Italy); Marcatili, Sara; Belcari, Nicola; Bisogni, Maria G. [University of Pisa and INFN Sezione di Pisa, I 56127 Pisa (Italy); Collazuol, Gianmaria [University of Padova and INFN Sezione di Padova (Italy); Ambrosi, Giovanni [INFN Sezione di Perugia, I 06100 Perugia (Italy); Corsi, Francesco; Foresta, Maurizio; Marzocca, Cristoforo; Matarrese, Gianvito [Politecnico di Bari and INFN Sezione di Bari, I 70100 Bari (Italy); Sportelli, Giancarlo; Guerra, Pedro; Santos, Andres [Universidad Politecnica de Madrid, E 28040 Madrid (Spain); Centro de Investigacion Biomedica en Red en Bioingenieria, Biomateriales y Nanomedicina (CIBER-BBN) (Spain); Del Guerra, Alberto [University of Pisa and INFN Sezione di Pisa, I 56127 Pisa (Italy)

    2012-12-11

    We are investigating the performances of a data acquisition system for Time of Flight PET, based on LYSO crystal slabs and 64 channels Silicon Photomultipliers matrices (1.2 cm{sup 2} of active area each). Measurements have been performed to test the timing capability of the detection system (SiPM matices coupled to a LYSO slab and the read-out electronics) with both test signal and radioactive source.

  16. Calibration and adjustment of the EGRET coincidence/time-of-flight system

    International Nuclear Information System (INIS)

    Hunter, S.D.

    1991-01-01

    The coincidence/time-of-flight system of the energetic gamma ray experiment telescope (EGRET) on NASA's Gamma Ray Observatory (GRO) consists of two layers of sixteen scintillator tiles. These tiles are paired into 96 coincidence telescopes. Valid coincidence and time-of-flight values (indicating downward moving particles) from one of these telescopes are two of the requirements for an EGRET event trigger. To maximize up-down discrimination, variations in the mean timing value of the telescopes must be minimized. The timing values of the 96 telescopes are not independent, hence they cannot be individually adjusted to calibrate the system. An iterative approach was devised to determine adjustments to the length of the photomultiplier signal cables. These adjustments were made directly in units of time using a time domain reflectometry technique, by timing the reflection of a fast pulse from the unterminated end of eable, and observing the charge in signal propagation time as the length of the cable was shortened. Two constant fraction discriminators, a time-to-amplitude converter and a pulse height analyzer were used for these measurements. Using this direct time measuring approach, the timing values for the 96 EGRET coincidence/time-of-flight telescopes were adjusted with an FWHM variation of less than 450 ps (± 1 TOF timing channel). (orig.)

  17. Determining the Time of Flight and Speed of Sound on Different types of Edible Oil

    Science.gov (United States)

    Azman, N. A.; Hamid, S. B. Abd

    2017-11-01

    Edible oil is most often plant-based oils that have been extracted from various seeds. There are cases where the fully virgin edible oil was found to be a fraud. The adulterated edible oil indicates the intentional, fraudulent addition of extraneous, improper or cheaper ingredients puts into the oil or the dilution or removal of some valuable ingredient of the oil in order to increase profits. Hence, decrease the reliability of the Malaysian food product quality. This research was done by using the method of time of flight obtained using the Texas Instrument board, TDC1000-TDC7200 EVM connected to an ultrasonic transducer with 1 MHz frequency. The authors measured the time of flight and temperatures controlled from 20°C to 40°C of five vegetable oils (olive oil, sunflower oil, corn oil, coconut oil, and mustard oil). The value is observed and compared with other research from the literature review. From the study, time of flight values decreases exponentially while speed of sound value increases. This relationship will be useful in spectrum unfolding method to investigate the adulteration in different type of edible oil.This research outcome is to investigate the quality value of the different type of edible oil while eliminates the issues where the quality of Malaysian food product is not reliable.

  18. Picosecond resolution on relativistic heavy ions' time-of-flight measurement

    Energy Technology Data Exchange (ETDEWEB)

    Ebran, A., E-mail: adeline.ebran@cea.fr; Taieb, J., E-mail: julien.taieb@cea.fr; Belier, G.; Chatillon, A.; Laurent, B.; Martin, J.-F.; Pellereau, E.

    2013-11-11

    We developed a time-of-flight measurement system for relativistic heavy ions with a requested resolution of 40 ps Full Width Half Maximum. Such a resolution is mandatory to assign the correct mass number to every fission fragment, identified using the Bρ-ToF-ΔE method with the recoil spectrometer designed for the SOFIA experiment—which hold very recently at GSI. To achieve such a performance, fast plastic scintillators read-out by dedicated photomultiplier tubes were chosen among other possible options. We have led several test-measurements from 2009 to 2011, in order to investigate: the effect of the addition of a quenching molecule in the scintillator's matrix, the influence of the detector's size and the impact of the photomultiplier tube. The contribution of the dedicated electronics is also characterized. Time-of-flight measurements were performed realized with electron pulses and relativistic heavy ions, respectively provided by the LASER driven electron–accelerator (ELSA) at CEA–DAM Ile-de-France and by the SIS18/FRS facility at GSI. The reported results exhibit a time resolution better than 20 ps Full Width Half Maximum reached with the last prototype at GSI with an Uranium beam. These results confirm that the SOFIA experiment should enable the measurement of the relativistic fission fragments' time-of-flight with the requested resolution.

  19. Picosecond resolution on relativistic heavy ions' time-of-flight measurement

    International Nuclear Information System (INIS)

    Ebran, A.; Taieb, J.; Belier, G.; Chatillon, A.; Laurent, B.; Martin, J.-F.; Pellereau, E.

    2013-01-01

    We developed a time-of-flight measurement system for relativistic heavy ions with a requested resolution of 40 ps Full Width Half Maximum. Such a resolution is mandatory to assign the correct mass number to every fission fragment, identified using the Bρ-ToF-ΔE method with the recoil spectrometer designed for the SOFIA experiment—which hold very recently at GSI. To achieve such a performance, fast plastic scintillators read-out by dedicated photomultiplier tubes were chosen among other possible options. We have led several test-measurements from 2009 to 2011, in order to investigate: the effect of the addition of a quenching molecule in the scintillator's matrix, the influence of the detector's size and the impact of the photomultiplier tube. The contribution of the dedicated electronics is also characterized. Time-of-flight measurements were performed realized with electron pulses and relativistic heavy ions, respectively provided by the LASER driven electron–accelerator (ELSA) at CEA–DAM Ile-de-France and by the SIS18/FRS facility at GSI. The reported results exhibit a time resolution better than 20 ps Full Width Half Maximum reached with the last prototype at GSI with an Uranium beam. These results confirm that the SOFIA experiment should enable the measurement of the relativistic fission fragments' time-of-flight with the requested resolution

  20. Using convolutional neural networks to estimate time-of-flight from PET detector waveforms

    Science.gov (United States)

    Berg, Eric; Cherry, Simon R.

    2018-01-01

    Although there have been impressive strides in detector development for time-of-flight positron emission tomography, most detectors still make use of simple signal processing methods to extract the time-of-flight information from the detector signals. In most cases, the timing pick-off for each waveform is computed using leading edge discrimination or constant fraction discrimination, as these were historically easily implemented with analog pulse processing electronics. However, now with the availability of fast waveform digitizers, there is opportunity to make use of more of the timing information contained in the coincident detector waveforms with advanced signal processing techniques. Here we describe the application of deep convolutional neural networks (CNNs), a type of machine learning, to estimate time-of-flight directly from the pair of digitized detector waveforms for a coincident event. One of the key features of this approach is the simplicity in obtaining ground-truth-labeled data needed to train the CNN: the true time-of-flight is determined from the difference in path length between the positron emission and each of the coincident detectors, which can be easily controlled experimentally. The experimental setup used here made use of two photomultiplier tube-based scintillation detectors, and a point source, stepped in 5 mm increments over a 15 cm range between the two detectors. The detector waveforms were digitized at 10 GS s-1 using a bench-top oscilloscope. The results shown here demonstrate that CNN-based time-of-flight estimation improves timing resolution by 20% compared to leading edge discrimination (231 ps versus 185 ps), and 23% compared to constant fraction discrimination (242 ps versus 185 ps). By comparing several different CNN architectures, we also showed that CNN depth (number of convolutional and fully connected layers) had the largest impact on timing resolution, while the exact network parameters, such as convolutional

  1. Quality control and identification of steroid saponins in crude extracts from Dioscorea zingiberensis C. H. Wright by fingerprint with HPLC-ELSD and HPLC-ESI-Quadrupole/Time-of-fight tandem mass spectrometry

    Science.gov (United States)

    Zhang, Xinxin; Liang, Jinru; Liu, Jianli; Zhao, Ye; Gao, Juan; Sun, Wenji; Ito, Yoichiro

    2014-01-01

    In this study, a fingerprint of steroid saponins, the major bioactive constituents in the crude extracts from Dioscorea zingiberensis C. H. Wright (DZW), has been established for the first time by high-performance liquid chromatography coupled with evaporative light scattering detector (HPLC-ELSD) and the simultaneous characterization of the steroid saponins by high-performance liquid chromatography coupled with electrospray ionization-mass spectrometry and quadrupole tandem time-of-fight mass analyzers detection (HPLC-ESI-Q/TOF). These HPLC analyses were both carried out on a Welchrom C18 column (250 mm × 4.6 mm I.D., 5 μm) with a mobile phase composed of water and acetonitrile under gradient elution. There were 68 common characteristic peaks in the fingerprints, in which 12 of them were confirmed by comparing their mass spectra and retention times with those of the reference compounds. In order to identify the other unknown peaks, their fragmentation behaviors characteristic for the major groups of steroid saponins from DZW with six types of aglycone skeletons were discussed in detail, and possible MS/MS fragmentation pathways were proposed for aiding the structural identification of these components. According to the summarized fragmentation patterns, these peaks were tentatively assigned by matching their empirical molecular formula with those of the published compounds, or by elucidating their quasi-molecular ions and fragment ions referring to available literature information when the reference standards were unavailable. As a result, 22 steroid saponins were found in DZW for the first time. In addition, the quantitative analysis of the 12 known peaks was accomplished at the same time which indicated that there was a great variability in the amount of these active compounds in different batches in the crude extracts. This approach could demonstrate that the fingerprint could be considered to be a suitable tool to comprehensively improve the quality control

  2. Triple quadrupole tandem mass spectrometry: A real alternative to high resolution magnetic sector instrument for the analysis of polychlorinated dibenzo-p-dioxins, furans and dioxin-like polychlorinated biphenyls.

    Science.gov (United States)

    García-Bermejo, Ángel; Ábalos, Manuela; Sauló, Jordi; Abad, Esteban; González, María José; Gómara, Belén

    2015-08-19

    This paper reports on the optimisation, characterisation, validation and applicability of gas chromatography coupled to triple quadrupole mass spectrometry in its tandem operation mode (GC-QqQ(MS/MS) for the quantification of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs, dioxins) and dioxin-like polychlorinated biphenyls (DL-PCBs) in environmental and food matrices. MS/MS parameters were selected to achieve the high sensitivity and selectivity required for the analysis of this type of compounds and samples. Good repeatability for areas (RSD = 1-10%, for PCDD/Fs and DL-PCBs) and for ion transition ratios (RSD = 0.3-10%, for PCDD/Fs, and 0.2-15%, for DL-PCBs) and low instrumental limits of detection, 0.07-0.75 pg μL(-1) (for dioxins) and 0.05-0.63 pg μL(-1) (for DL-PCBs), were obtained. A comparative study of the congener specific determination using both GC-QqQ(MS/MS) and gas chromatography-high resolution mass spectrometry (GC-HRMS) was also performed by analysing several fortified samples and certified reference materials (CRMs) with low (feed and foodstuffs), median (sewage sludge) and high (fly ash) toxic equivalency (TEQ) concentration levels, i.e. 0.60, 1.83, 72.9 and 3609 pg WHO-TEQ(PCDD/Fs) g(-1). The agreement between the results obtained for the total TEQs (dioxins) on GC-QqQ(MS/MS) and GC-HRMS in all the investigated samples were within the range of ±4%, and that of DL-PCBs at concentration levels of 0.84 pg WHO-TEQs (DL-PCBs) g(-1), in the case of feedstuffs, was 0.11%. Both instrumental methods have similar and comparable linearity, precision and accuracy. The GC-QqQ(MS/MS) sensitivity, lower than that of GC-HRMS, is good enough (iLODs in the down to low pg levels) to detect the normal concentrations of these compounds in food and environmental samples. These results make GC-QqQ(MS/MS) suitable for the quantitative analysis of dioxins and DL-PCBs and a real alternative tool to the reference sector HRMS instruments. Copyright © 2015 Elsevier

  3. Fully automatic and precise data analysis developed for time-of-flight mass spectrometry.

    Science.gov (United States)

    Meyer, Stefan; Riedo, Andreas; Neuland, Maike B; Tulej, Marek; Wurz, Peter

    2017-09-01

    Scientific objectives of current and future space missions are focused on the investigation of the origin and evolution of the solar system with the particular emphasis on habitability and signatures of past and present life. For in situ measurements of the chemical composition of solid samples on planetary surfaces, the neutral atmospheric gas and the thermal plasma of planetary atmospheres, the application of mass spectrometers making use of time-of-flight mass analysers is a technique widely used. However, such investigations imply measurements with good statistics and, thus, a large amount of data to be analysed. Therefore, faster and especially robust automated data analysis with enhanced accuracy is required. In this contribution, an automatic data analysis software, which allows fast and precise quantitative data analysis of time-of-flight mass spectrometric data, is presented and discussed in detail. A crucial part of this software is a robust and fast peak finding algorithm with a consecutive numerical integration method allowing precise data analysis. We tested our analysis software with data from different time-of-flight mass spectrometers and different measurement campaigns thereof. The quantitative analysis of isotopes, using automatic data analysis, yields results with an accuracy of isotope ratios up to 100 ppm for a signal-to-noise ratio (SNR) of 10 4 . We show that the accuracy of isotope ratios is in fact proportional to SNR -1 . Furthermore, we observe that the accuracy of isotope ratios is inversely proportional to the mass resolution. Additionally, we show that the accuracy of isotope ratios is depending on the sample width T s by T s 0.5 . Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  4. Quasi-dynamic mode of nanomembranes for time-of-flight mass spectrometry of proteins.

    Science.gov (United States)

    Park, Jonghoo; Kim, Hyunseok; Blick, Robert H

    2012-04-21

    Mechanical resonators realized on the nano-scale by now offer applications in mass-sensing of biomolecules with extraordinary sensitivity. The general idea is that perfect mechanical biosensors should be of extremely small size to achieve zeptogram sensitivity in weighing single molecules similar to a balance. However, the small scale and long response time of weighing biomolecules with a cantilever restrict their usefulness as a high-throughput method. Commercial mass spectrometry (MS) such as electro-spray ionization (ESI)-MS and matrix-assisted laser desorption/ionization (MALDI)-time of flight (TOF)-MS are the gold standards to which nanomechanical resonators have to live up to. These two methods rely on the ionization and acceleration of biomolecules and the following ion detection after a mass selection step, such as time-of-flight (TOF). Hence, the spectrum is typically represented in m/z, i.e. the mass to ionization charge ratio. Here, we describe the feasibility and mass range of detection of a new mechanical approach for ion detection in time-of-flight mass spectrometry, the principle of which is that the impinging ion packets excite mechanical oscillations in a silicon nitride nanomembrane. These mechanical oscillations are henceforth detected via field emission of electrons from the nanomembrane. Ion detection is demonstrated in MALDI-TOF analysis over a broad range with angiotensin, bovine serum albumin (BSA), and an equimolar protein mixture of insulin, BSA, and immunoglobulin G (IgG). We find an unprecedented mass range of operation of the nanomembrane detector.

  5. A neutron time of flight spectrometer appropriate for D-T plasma diagnostics

    International Nuclear Information System (INIS)

    Elevant, T.

    1984-02-01

    A neutron time-of-flight spectrometer with 2 m flight path for diagnostics of deuterium plasmas in JET is presently under construction. An upgrade of this spectrometer to make it appropriate for 14-MeV neutron spectroscopy is presented here. It is suggested to use backscattering in a deuterium based scintillator. The flight path length is 1-2 m and the efficiency is of the order of 2.10 -5 cm -5 . Results from test of principle are presented with estimates for neutron and gamma backgrounds

  6. Time-of-Flight Three Dimensional Neutron Diffraction in Transmission Mode for Mapping Crystal Grain Structures

    DEFF Research Database (Denmark)

    Cereser, Alberto; Strobl, Markus; Hall, Stephen A.

    2017-01-01

    constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND......-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure...

  7. Time lens for high-resolution neutron time-of-flight spectrometers

    International Nuclear Information System (INIS)

    Baumann, K.; Gaehler, R.; Grigoriev, P.; Kats, E.I.

    2005-01-01

    We examine in analytic and numeric ways the imaging effects of temporal neutron lenses created by traveling magnetic fields. For fields of parabolic shape we derive the imaging equations, investigate the time magnification, the evolution of the phase-space element, the gain factor, and the effect of finite beam size. The main aberration effects are calculated numerically. The system is technologically feasible and should convert neutron time-of-flight instruments from pinhole to imaging configuration in time, thus enhancing intensity and/or time resolution. Further fields of application for high-resolution spectrometry may be opened

  8. A high performance Time-of-Flight detector applied to isochronous mass measurement at CSRe

    International Nuclear Information System (INIS)

    Mei Bo; Tu Xiaolin; Wang Meng; Xu Hushan; Mao Ruishi; Hu Zhengguo; Ma Xinwen; Yuan Youjin; Zhang Xueying; Geng Peng; Shuai Peng; Zang Yongdong; Tang Shuwen; Ma Peng; Lu Wan; Yan Xinshuai; Xia Jiawen; Xiao Guoqing; Guo Zhongyan; Zhang Hongbin

    2010-01-01

    A high performance Time-of-Flight detector has been designed and constructed for isochronous mass spectrometry at the experimental Cooler Storage Ring (CSRe). The detector has been successfully used in an experiment to measure the masses of the N∼Z∼33 nuclides near the proton drip-line. Of particular interest is the mass of 65 As. A maximum detection efficiency of 70% and a time resolution of 118±8 ps (FWHM) have been achieved in the experiment. The dependence of detection efficiency and signal average pulse height (APH) on atomic number Z has been studied. The potential of APH for Z identification has been discussed.

  9. Improved measurement linearity and precision for AMCW time-of-flight range imaging cameras.

    Science.gov (United States)

    Payne, Andrew D; Dorrington, Adrian A; Cree, Michael J; Carnegie, Dale A

    2010-08-10

    Time-of-flight range imaging systems utilizing the amplitude modulated continuous wave (AMCW) technique often suffer from measurement nonlinearity due to the presence of aliased harmonics within the amplitude modulation signals. Typically a calibration is performed to correct these errors. We demonstrate an alternative phase encoding approach that attenuates the harmonics during the sampling process, thereby improving measurement linearity in the raw measurements. This mitigates the need to measure the system's response or calibrate for environmental changes. In conjunction with improved linearity, we demonstrate that measurement precision can also be increased by reducing the duty cycle of the amplitude modulated illumination source (while maintaining overall illumination power).

  10. Neutron time-of-flight techniques for investigation of the extinction effect

    International Nuclear Information System (INIS)

    Niimura, N.; Tomiyoshi, S.; Takahashi, J.; Harada, J.

    1975-01-01

    An application of the time-of-flight neutron diffraction technique to an investigation of the nature of the extinction effect in a single-crystal specimen is given. It is shown that the wavelength dependence of the extinction can be easily obtained by changing the scattering angle. An estimation of the extinction factor for a CuCl single crystal is given as an example and a comparison of the results with recent extinction theory [Becker and Coppens. Acta Cryst.(1974). A30, 129-147; 148-153] is made. (Auth.)

  11. A time-of-flight array for 1 to 2 GeV/c particles

    International Nuclear Information System (INIS)

    Sum, V.; Berdoz, A.R.; Davis, C.A.

    1992-09-01

    A time-of-flight detector array has been developed for an experiment searching for the strangeness -2 H-particle. The array consists of 40 logs of plastic scintillator with dimensions 2.00 x 0.085 x 0.050 m 3 . The photomultiplier tubes are coupled to the scintillators without the use of light guides, and the mounting of the bars is designed for easy adjustment and servicing. The average intrinsic time resolution was found to be 110 ps σ. 8 refs., 9 figs., 1 tab

  12. Indoor and Outdoor Depth Imaging of Leaves With Time-of-Flight and Stereo Vision Sensors

    DEFF Research Database (Denmark)

    Kazmi, Wajahat; Foix, Sergi; Alenya, Guilliem

    2014-01-01

    In this article we analyze the response of Time-of-Flight (ToF) cameras (active sensors) for close range imaging under three different illumination conditions and compare the results with stereo vision (passive) sensors. ToF cameras are sensitive to ambient light and have low resolution but deliver...... poorly under sunlight. Stereo vision is comparatively more robust to ambient illumination and provides high resolution depth data but is constrained by texture of the object along with computational efficiency. Graph cut based stereo correspondence algorithm can better retrieve the shape of the leaves...

  13. Time-of-flight camera via a single-pixel correlation image sensor

    Science.gov (United States)

    Mao, Tianyi; Chen, Qian; He, Weiji; Dai, Huidong; Ye, Ling; Gu, Guohua

    2018-04-01

    A time-of-flight imager based on single-pixel correlation image sensors is proposed for noise-free depth map acquisition in presence of ambient light. Digital micro-mirror device and time-modulated IR-laser provide spatial and temporal illumination on the unknown object. Compressed sensing and ‘four bucket principle’ method are combined to reconstruct the depth map from a sequence of measurements at a low sampling rate. Second-order correlation transform is also introduced to reduce the noise from the detector itself and direct ambient light. Computer simulations are presented to validate the computational models and improvement of reconstructions.

  14. Software of structure experiMents in a neutron time-of-flight diffractometer

    International Nuclear Information System (INIS)

    Balagurov, A.M.; Dlouga, M.; Zlokazov, V.B.; Mironova, G.M.

    1978-01-01

    A set of programs is discussed to be used in diffraction experiment in a neutron time-of-flight diffractometer. The DIFRAT program, which processes spectra of poly and monocrystals, locates all spectrum maxima and assesses their width on the basis of given experimental data and elementary cell parameters. Accurate location of maxima, evaluation of their area and width is done by the IREAK program. The most important feature of this program is a capability to set an experimental model of maxima patterns. The EXPDAT program is developed to investigate structural characteristics of a sample. It calculates corrections for absorbtion and extinction

  15. A time-of-flight neutron reflectometer for surface and interfacial studies

    International Nuclear Information System (INIS)

    Penfold, J.; Ward, R.C.; Williams, W.G.

    1987-03-01

    A time-of-flight neutron reflectometer constructed for surface and interfacial studies, and installed at the ISIS pulsed neutron source, is described. One of its important design features is its inclined incident beam, since this allows both liquid and solid surface phenomena to be investigated. Measurements are presented to show the performance of the instrument, and new representative results, which include studies of liquid surfaces, Langmuir-Blodgett films, and thin film multilayers, are included as illustrations of the scientific potential of the method. (author)

  16. High resolution time-of-flight spectrometer for crossed molecular beam study of elementary chemical reactions

    International Nuclear Information System (INIS)

    Qiu Minghui; Che Li; Ren Zefeng; Dai Dongxu; Wang Xiuyan; Yang Xueming

    2005-01-01

    In this article, we describe an apparatus in our laboratory for investigating elementary chemical reactions using the high resolution time-of-flight Rydberg tagging method. In this apparatus, we have adopted a rotating source design so that collision energy can be changed for crossed beam studies of chemical reactions. Preliminary results on the HI photodissociation and the F atom reaction with H 2 are reported here. These results suggest that the experimental apparatus is potentially a powerful tool for investigating state-to-state dynamics of elementary chemical reactions

  17. Calibration of the time response functions of a quenched plastic scintillator for neutron time of flight

    CERN Document Server

    Chen, J B; Peng, H S; Tang, C H; Zhang, B H; Ding, Y K; Chen, M; Chen, H S; Li, C G; Wen, T S; Yu, R Z

    2002-01-01

    The time response functions of an ultrafast quenched plastic scintillation detector used to measure neutron time of flight spectra were calibrated by utilizing cosmic rays and implosion neutrons from DT-filled capsules at the Shenguang II laser facility. These sources could be regarded as delta function pulses due to their much narrower time widths than those of the time response functions of the detection system. The results showed that the detector responses to DT neutrons and to cosmic rays were 1.18 and 0.96 ns FWHM, respectively.

  18. A silicon photomultiplier readout for time of flight neutron spectroscopy with {gamma}-ray detectors

    Energy Technology Data Exchange (ETDEWEB)

    Pietropaolo, A.; Gorini, G. [Dipartimento di Fisica ' ' G. Occhialini' ' and CNISM, Universita Degli Studi di Milano-Bicocca, Piazza della Scienza 3, 20126 Milano (Italy); Festa, G.; Andreani, C.; De Pascale, M. P.; Reali, E. [Dipartimento di Fisica and Centro NAST, Universita degli Studi di Roma Tor Vergata, Via della Ricerca Scientifica 1, 00133, Roma (Italy); Grazzi, F. [Istituto dei Sistemi Complessi-Consiglio Nazionale delle Ricerche, Via Madonna del Piano n.10, I-50019 Sesto Fiorentino, Firenze (Italy); Schooneveld, E. M. [ISIS Facility, Rutherford Appleton Laboratory, Chilton, Didcot, Oxfordshire, OX11 0QX (United Kingdom)

    2009-09-15

    The silicon photomultiplier (SiPM) is a recently developed photosensor used in particle physics, e.g., for detection of minimum ionizing particles and/or Cherenkov radiation. Its performance is comparable to that of photomultiplier tubes, but with advantages in terms of reduced volume and magnetic field insensitivity. In the present study, the performance of a gamma ray detector made of an yttrium aluminum perovskite scintillation crystal and a SiPM-based readout is assessed for use in time of flight neutron spectroscopy. Measurements performed at the ISIS pulsed neutron source demonstrate the feasibility of {gamma}-detection based on the new device.

  19. New development for the reverse time of flight analysis of spectra measured using Fourier Diffractometer Facilities

    CERN Document Server

    Maayouf, R M A

    2002-01-01

    The present work introduces a new design to replace the (Finnish make) reverse time of flight (RTOF) analyzer used for the Fourier diffractometer facilities. The new design applies a data acquisition system, a special interface card and software program installed in a PC computer, to perform the cross-correlation functions between signals received from the chopper-decoder and detector. It has been found from test measurements performed with the Cairo Fourier diffractometer facility (CFDF) and the similar high resolution one at JINR (Dubna-Russia) that the new design can successfully replace the Finnish make RTOF analyzer.

  20. Rotation stability of high speed neutron time-of-flight mechanical chopper

    International Nuclear Information System (INIS)

    Habib, N.; Adib, M.

    1998-01-01

    A modified rotation stabilization system has been designed to maintain the stability of a neutron time-of-flight (TOF) mechanical chopper rates from 460 rpm to 16000 rpm. The main principle of the system is based on comparing the chopper's rotation period with the preselected one from a quartz timer. The result of comparison is used to control the current driver of the chopper's motor. A 600 Hz three phase generator controlled by a magnetic amplifier was used as a current driver. The stability of the chopper's rotation rate at 16000 rpm was 0.02%. An improved method precise time scale calibration of the TOF spectrometer is applied

  1. Timing Calibration for Time-of-Flight PET Using Positron-Emitting Isotopes and Annihilation Targets

    Science.gov (United States)

    Li, Xiaoli; Burr, Kent C.; Wang, Gin-Chung; Du, Huini; Gagnon, Daniel

    2016-06-01

    Adding time-of-flight (TOF) technology has been proven to improve image quality in positron emission tomography (PET). In order for TOF information to significantly reduce the statistical noise in reconstructed PET images, good timing resolution is needed across the scanner field of view (FOV). This work proposes an accurate, robust, and practical crystal-based timing calibration method using 18F - FDG positron-emitting sources together with a spatially separated annihilation target. We calibrated a prototype Toshiba TOF PET scanner using this method and then assessed its timing resolution at different locations in the scanner FOV.

  2. Use of a large time-compensated scintillation detector in neutron time-of-flight measurements

    International Nuclear Information System (INIS)

    Goodman, C.D.

    1979-01-01

    A scintillator for neutron time-of-flight measurements is positioned at a desired angle with respect to the neutron beam, and as a function of the energy thereof, such that the sum of the transit times of the neutrons and photons in the scintillator are substantially independent of the points of scintillations within the scintillator. Extrapolated zero timing is employed rather than the usual constant fraction timing. As a result, a substantially larger scintillator can be employed that substantially increases the data rate and shortens the experiment time. 3 claims

  3. New developments in molecular imaging: positron emission tomography time-of-flight (TOF-PET)

    International Nuclear Information System (INIS)

    Aguilar, P.; Couce, B.; Iglesias, A.; Lois, C.

    2011-01-01

    Positron Emission tomography (PET) in increasingly being used in oncology for the diagnosis and staging of disease, as well as in monitoring response to therapy. One of the last advances in PET is the incorporation of Time-of-Flight (TOF) information, which improves the tomographic reconstruction process and subsequently the quality of the final image. In this work, we explain the principles of PET and the fundamentals of TOF-PET. Clinical images are shown in order to illustrate how TOF-PET improves the detectability of small lesions, particularly in patients with high body mass index. (Author) 20 refs

  4. FOCUS: time-of-flight spectrometer for cold neutrons at SINQ

    Energy Technology Data Exchange (ETDEWEB)

    Janssen, S; Mesot, J [Lab. for Neutron Scattering ETH Zurich, Zurich (Switzerland) and Paul Scherrer Institute, Villigen (Switzerland); Hempelmann, R [Saarbruecken Univ., Physical Chemistry, Saarbruecken (Germany)

    1996-11-01

    The physical layout of the Time-Of-Flight spectrometer at the new spallation source SINQ is presented. The concept shows up a hybrid-TOF combining a Fermi-chopper with a crystal monochromator. The demand of a versatile and flexible instrument for several applications is taken into account by the option of switching from time-focusing to monochromatic focusing mode such that the spectrometer can be optimised for both quasielastic and inelastic scattering applications. (author) 5 figs., 2 tabs., 16 refs.

  5. Measurement of detector neutron energy response using time-of-flight techniques

    International Nuclear Information System (INIS)

    Janee, H.S.

    1973-09-01

    The feasibility of using time-of-flight techniques at the EG and G/AEC linear accelerator for measuring the neutron response of relatively sensitive detectors over the energy range 0.5 to 14 MeV has been demonstrated. The measurement technique is described in detail as are the results of neutron spectrum measurements from beryllium and uranium photoneutron targets. The sensitivity of a fluor photomultiplier LASL detector with a 2- by 1-inch NE-111 scintillator was determined with the two targets, and agreement in the region of overlap was very good. (U.S.)

  6. A study of aging effects of barrel Time-Of-Flight system in the BESIII experiment

    Science.gov (United States)

    Liu, Huan-Huan; Sun, Sheng-Sen; Fang, Shuang-Shi; Wu, Zhi; Dai, Hong-Liang; Heng, Yue-Kun; Zhou, Ming; Deng, Zi-Yan; Liu, Huai-Min

    2018-02-01

    The Time-Of-Flight system consisting of plastic scintillation counters plays an important role for particle identification in the BESIII experiment at the BEPCII double ring e+e- collider. Degradation of the detection efficiency of the barrel TOF system has been observed since the start of physical data taking and this effect has triggered intensive and systematic studies about aging effects of the detector. The aging rates of the attenuation lengths and relative gains are obtained based on the data acquired in past several years. This study is essential for ensuring an extended operation of the barrel TOF system in optimal conditions.

  7. Energy measurement using a resonator-based time-of-flight system

    International Nuclear Information System (INIS)

    Pardo, R.C.; Lewis, R.N.; Johnson, K.W.; Clifft, B.

    1983-01-01

    The resonant time-of-flight system which has been developed has several advantages over other potential approaches. The system is non-interceptive and nondestructive. The beam phase space is preserved. It is non-dispersive. Path length variations are not introduced into the beam transport which would reduce the timing resolution. It has a large signal-to-noise ratio when compared to non-resonant beam pick-up techniques. It provides the means to precisely set the linac energy and, potentially, to control the energy in a feedback loop is desired. It is less expensive than an equivalent magnetic system

  8. Double-arm time-of-flight mass-spectrometer of nuclear fragments

    International Nuclear Information System (INIS)

    Ajvazian, G.M.; Astabatyan, R.A.

    1995-01-01

    A double-arm time-of-flight spectrometer of nuclear fragments for the investigation of heavy nuclei photofission in the intermediate energy range is described. The calibration results and working characteristics of the spectrometer, obtained using 252 Cf as a source of spontaneous fission, are presented. A mass resolution of σ m ∼2-3 a.m.u. was obtained within the registered fragments mass range of 80-160 a.m.u. The spectrometer was tested in the experiment on the investigation of 238 U nuclei fission by Bremsstahlung photons with Eγ max=1.75 GeV

  9. Environmental Effects on Measurement Uncertainties of Time-of-Flight Cameras

    DEFF Research Database (Denmark)

    Gudmundsson, Sigurjon Arni; Aanæs, Henrik; Larsen, Rasmus

    2007-01-01

    In this paper the effect the environment has on the SwissRanger SR3000 Time-Of-Flight camera is investigated. The accuracy of this camera is highly affected by the scene it is pointed at: Such as the reflective properties, color and gloss. Also the complexity of the scene has considerable effects...... on the accuracy. To mention a few: The angle of the objects to the emitted light and the scattering effects of near objects. In this paper a general overview of known such inaccuracy factors are described, followed by experiments illustrating the additional uncertainty factors. Specifically we give a better...

  10. Testing a new NIF neutron time-of-flight detector with a bibenzyl scintillator on OMEGA.

    Science.gov (United States)

    Glebov, V Yu; Forrest, C; Knauer, J P; Pruyne, A; Romanofsky, M; Sangster, T C; Shoup, M J; Stoeckl, C; Caggiano, J A; Carman, M L; Clancy, T J; Hatarik, R; McNaney, J; Zaitseva, N P

    2012-10-01

    A new neutron time-of-flight (nTOF) detector with a bibenzyl crystal as a scintillator has been designed and manufactured for the National Ignition Facility (NIF). This detector will replace a nTOF20-Spec detector with an oxygenated xylene scintillator currently operational on the NIF to improve the areal-density measurements. In addition to areal density, the bibenzyl detector will measure the D-D and D-T neutron yield and the ion temperature of indirect- and direct-drive-implosion experiments. The design of the bibenzyl detector and results of tests on the OMEGA Laser System are presented.

  11. A mechanical nanomembrane detector for time-of-flight mass spectrometry.

    Science.gov (United States)

    Park, Jonghoo; Qin, Hua; Scalf, Mark; Hilger, Ryan T; Westphall, Michael S; Smith, Lloyd M; Blick, Robert H

    2011-09-14

    We describe here a new principle for ion detection in time-of-flight (TOF) mass spectrometry in which an impinging ion packet excites mechanical vibrations in a silicon nitride (Si(3)N(4)) nanomembrane. The nanomembrane oscillations are detected by means of time-varying field emission of electrons from the mechanically oscillating nanomembrane. Ion detection is demonstrated in the MALDI-TOF analysis of proteins varying in mass from 5729 (insulin) to 150,000 (Immunoglobulin G) daltons. The detector response agrees well with the predictions of a thermomechanical model in which the impinging ion packet causes a nonuniform temperature distribution in the nanomembrane, exciting both fundamental and higher order oscillations.

  12. Gas Time-of-Flight Cherenkov Detector with Radiofrequency Phototube for FP420

    International Nuclear Information System (INIS)

    Margaryan, A.

    2011-01-01

    In this paper, the gas Cherenkov detector with radiofrequency phototube is considered as a fast-timing detector for FP420 project. The detector serves for precise Time-of-Flight measurements of forward going protons, capable of accurate vertex reconstruction and background rejection at high luminosities. The proposed technique is a high resolution (∼ 5 ps FWHM for a single proton), high rate (∼ MHz) and highly stable (less than 1 ps) timing technique capable to detect up to several tens events in a short (∼ 1 ns) time interval. (author)

  13. A time-of-flight array for 1 to 2 GeV/c particles

    Energy Technology Data Exchange (ETDEWEB)

    Sum, V; Berdoz, A R; Davis, C A [Manitoba Univ., Winnipeg, MB (Canada). Dept. of Physics; and others

    1992-09-01

    A time-of-flight detector array has been developed for an experiment searching for the strangeness -2 H-particle. The array consists of 40 logs of plastic scintillator with dimensions 2.00 x 0.085 x 0.050 m{sup 3}. The photomultiplier tubes are coupled to the scintillators without the use of light guides, and the mounting of the bars is designed for easy adjustment and servicing. The average intrinsic time resolution was found to be 110 ps {sigma}. 8 refs., 9 figs., 1 tab.

  14. A time-of-flight system for precise measurements of a relativistic charged particle beam momentum

    International Nuclear Information System (INIS)

    Avramenko, S.A.; Belikov, Yu.A.; Golokhvastov, A.I.; Lukstin'sh, Yu.; Man'yakov, P.K.; Rukoyatkin, P.A.; Khorozov, S.A.

    1996-01-01

    A time-of-flight system with a time resolution (σ) about 100 ps is described. The methods for the calibration, stability verification and the method for the time resolution evaluation in conditions of a nonmonochromatic beam are discussed especially. The system was applied in charge exchange ( 3 H, 3 He) experiments with the GIBS spectrometer for a measurement of 3 H-nuclei momenta at 2 GeV/c per nucleon with a precision about 0.2%. (author). 4 refs., 7 figs., 1 tab

  15. Ultrasonic divergent-beam scanner for time-of-flight tomography with computer evaluation

    Energy Technology Data Exchange (ETDEWEB)

    Glover, G H

    1978-03-02

    The rotatable ultrasonic divergent-beam scanner is designed for time-of-flight tomography with computer evaluation. With it there can be measured parameters that are of importance for the structure of soft tissues, e.g. time as a function of the velocity distribution along a certain path of flight(the method is analogous to the transaxial X-ray tomography). Moreover it permits to perform the quantitative measurement of two-dimensional velocity distributions and may therefore be applied to serial examinations for detecting cancer of the breast. As computers digital memories as well as analog-digital-hybrid systems are suitable.

  16. Calibration of time of flight detectors using laser-driven neutron source

    Energy Technology Data Exchange (ETDEWEB)

    Mirfayzi, S. R.; Kar, S., E-mail: s.kar@qub.ac.uk; Ahmed, H.; Green, A.; Alejo, A.; Jung, D. [Centre for Plasma Physics, School of Mathematics and Physics, Queen’s University Belfast, Belfast BT7 1NN (United Kingdom); Krygier, A. G.; Freeman, R. R. [Department of Physics, The Ohio State University, Columbus, Ohio 43210 (United States); Clarke, R. [Central Laser Facility, Rutherford Appleton Laboratory, Didcot, Oxfordshire OX11 0QX (United Kingdom); Fuchs, J.; Vassura, L. [LULI, Ecole Polytechnique, CNRS, Route de Saclay, 91128 Palaiseau Cedex (France); Kleinschmidt, A.; Roth, M. [Institut für Kernphysik, Technische Universität Darmstadt, Schloßgartenstrasse 9, D-64289 Darmstadt,Germany (Germany); Morrison, J. T. [Propulsion Systems Directorate, Air Force Research Lab, Wright Patterson Air Force Base, Ohio 45433 (United States); Najmudin, Z.; Nakamura, H. [Blackett Laboratory, Department of Physics, Imperial College, London SW7 2AZ (United Kingdom); Norreys, P. [Central Laser Facility, Rutherford Appleton Laboratory, Didcot, Oxfordshire OX11 0QX (United Kingdom); Department of Physics, University of Oxford, Oxford OX1 3PU (United Kingdom); Oliver, M. [Department of Physics, University of Oxford, Oxford OX1 3PU (United Kingdom); Zepf, M. [Centre for Plasma Physics, School of Mathematics and Physics, Queen’s University Belfast, Belfast BT7 1NN (United Kingdom); Helmholtz Institut Jena, D-07743 Jena (Germany); Borghesi, M. [Centre for Plasma Physics, School of Mathematics and Physics, Queen’s University Belfast, Belfast BT7 1NN (United Kingdom); Institute of Physics of the ASCR, ELI-Beamlines Project, Na Slovance 2, 18221 Prague (Czech Republic)

    2015-07-15

    Calibration of three scintillators (EJ232Q, BC422Q, and EJ410) in a time-of-flight arrangement using a laser drive-neutron source is presented. The three plastic scintillator detectors were calibrated with gamma insensitive bubble detector spectrometers, which were absolutely calibrated over a wide range of neutron energies ranging from sub-MeV to 20 MeV. A typical set of data obtained simultaneously by the detectors is shown, measuring the neutron spectrum emitted from a petawatt laser irradiated thin foil.

  17. Calibration of time of flight detectors using laser-driven neutron source

    Science.gov (United States)

    Mirfayzi, S. R.; Kar, S.; Ahmed, H.; Krygier, A. G.; Green, A.; Alejo, A.; Clarke, R.; Freeman, R. R.; Fuchs, J.; Jung, D.; Kleinschmidt, A.; Morrison, J. T.; Najmudin, Z.; Nakamura, H.; Norreys, P.; Oliver, M.; Roth, M.; Vassura, L.; Zepf, M.; Borghesi, M.

    2015-07-01

    Calibration of three scintillators (EJ232Q, BC422Q, and EJ410) in a time-of-flight arrangement using a laser drive-neutron source is presented. The three plastic scintillator detectors were calibrated with gamma insensitive bubble detector spectrometers, which were absolutely calibrated over a wide range of neutron energies ranging from sub-MeV to 20 MeV. A typical set of data obtained simultaneously by the detectors is shown, measuring the neutron spectrum emitted from a petawatt laser irradiated thin foil.

  18. Calibration of time of flight detectors using laser-driven neutron source

    International Nuclear Information System (INIS)

    Mirfayzi, S. R.; Kar, S.; Ahmed, H.; Green, A.; Alejo, A.; Jung, D.; Krygier, A. G.; Freeman, R. R.; Clarke, R.; Fuchs, J.; Vassura, L.; Kleinschmidt, A.; Roth, M.; Morrison, J. T.; Najmudin, Z.; Nakamura, H.; Norreys, P.; Oliver, M.; Zepf, M.; Borghesi, M.

    2015-01-01

    Calibration of three scintillators (EJ232Q, BC422Q, and EJ410) in a time-of-flight arrangement using a laser drive-neutron source is presented. The three plastic scintillator detectors were calibrated with gamma insensitive bubble detector spectrometers, which were absolutely calibrated over a wide range of neutron energies ranging from sub-MeV to 20 MeV. A typical set of data obtained simultaneously by the detectors is shown, measuring the neutron spectrum emitted from a petawatt laser irradiated thin foil

  19. Design study of a time-of-flight neutron spectrometer for JT-60U

    International Nuclear Information System (INIS)

    Elevant, T.; Hoek, M.; Nishitani, Takeo.

    1993-06-01

    A time-of-flight neutron spectrometer is proposed for measurements of neutron energy spectra from deuterium-deuterium reactions in JT-60U tokamak plasmas. The sensitivity of the instrument is 2 · 10 -2 cm 2 , energy resolution is 4.5 % (FWHM) and maximum useful count-rate is 6 kHz. Analysis of neutron energy spectra will provide information on central ion temperatures larger than ∼ 4 keV with an accuracy of ± 10 %, and neutron source fraction from reactions between thermal ions with an accuracy of ± 15 %. The minimum time required for data acquisition is 0.1 s. (author)

  20. Clock-transport synchronisation for neutrino time-of-flight measurements

    International Nuclear Information System (INIS)

    Field, J.H.

    2012-01-01

    A method to synchronise, at the sub-nanosecond level, clocks used for neutrino time-of-flight measurements is proposed. Clocks situated near the neutrino source and target are compared with a moveable clock that is transported between them. The general-relativistic theory of the procedure was tested and verified in an experiment performed by Hafele and Keating in 1972. It is suggested that use of such a synchronisation method may contribute to a precise test of the Sagnac effect - a measured velocity greater than c - for neutrinos of the proposed LBNE beam between Fermilab and the Homestake mine. (orig.)

  1. Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Nielen, M W; Buijtenhuijs, F A

    1999-05-01

    Hyphenation of liquid chromatography (LC) techniques with electrospray ionization (ESI) orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS) provides both MS-based structural information and LC-based quantitative data in polymer analysis. In one experimental setup, three different LC modes are interfaced with MS:  size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS). In SEC/MS, both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra are achieved. GPEC/MS shows detailed chemical heterogeneity of the polymer and the chemical composition distribution within oligomer groups. In LCCC/MS, the retention behavior is primarily governed by chemical heterogeneities, such as different end group functionalities, and quantitative end group calculations can be easily made. The potential of these methods and the benefit of time-of-flight analyzers in polymer analysis are discussed using SEC/MS of a polydisperse poly(methyl methacrylate) sample, GPEC/MS of dipropoxylated bisphenol A/adipic acid polyester resin, LCCC/MS of alkylated poly(ethylene glycol), and LCCC/MS of terephthalic acid/neopentyl glycol polyester resin.

  2. Electric field measurement in the ionosphere using the time-of-flight technique

    International Nuclear Information System (INIS)

    Nakamura, Masato; Hayakawa, Hajime; Tsuruda, Koichiro

    1989-01-01

    The first successful electric field measurement in the ionosphere using the time-of-flight technique with a lithium ion beam was carried out on a S-520 sounding rocket launched from Kagoshima Space Center, Japan on January 15, 1987. The purpose of this experiment was to prove the validity of the time-of-flight technique when it is applied to the measurement of the dc electric field in the ionosphere. A time-coded ion beam was ejected from the rocket in the direction perpendicular to the Earth's magnetic field. The beam returned to the rocket twice per rocket spin when the initial beam direction was nearly perpendicular to the electric field. The electric field and the magnetic field were derived from the travel time of these return lithium ions. The accuracy of the electric field determination was ± 0.3 mV/m. The direction of the electric field was obtained from the direction of the returning ion beam after about one ion gyration. The main constituent of the measured electric field was a V x B field due to the rocket motion across the geomagnetic field. The ambient field was less than 1 mV/m. The magnetic field was measured with an accuracy of ± 2.7 nT in this experiment

  3. Barrel time-of-flight detector for the PANDA experiment at FAIR

    Science.gov (United States)

    Gruber, L.; Brunner, S. E.; Marton, J.; Orth, H.; Suzuki, K.; PANDA Tof Group

    2016-07-01

    The barrel time-of-flight detector for the PANDA experiment at FAIR is foreseen as a Scintillator Tile (SciTil) Hodoscope based on several thousand small plastic scintillator tiles read-out with directly attached Silicon Photomultipliers (SiPMs). The main tasks of the system are an accurate determination of the time origin of particle tracks to avoid event mixing at high collision rates, relative time-of-flight measurements as well as particle identification in the low momentum regime. The main requirements are the use of a minimum material amount and a time resolution of σ < 100 ps. We have performed extensive optimization studies and prototype tests to prove the feasibility of the SciTil design and finalize the R&D phase. In a 2.7 GeV/c proton beam at Forschungszentrum Jülich a time resolution of about 80 ps has been achieved using SiPMs from KETEK and Hamamatsu with an active area of 3 × 3mm2. Employing the Digital Photon Counter from Philips a time resolution of about 30 ps has been reached.

  4. TOFPET 2: A high-performance circuit for PET time-of-flight

    Energy Technology Data Exchange (ETDEWEB)

    Di Francesco, Agostino, E-mail: agodifra@lip.pt [LIP, Lisbon (Portugal); Bugalho, Ricardo [LIP, Lisbon (Portugal); PETsys Electronics, Oeiras (Portugal); Oliveira, Luis [CTS-UNINOVA, DEE FCT-UNL, Caparica (Portugal); Rivetti, Angelo [INFN - sez. Torino (Italy); Rolo, Manuel [LIP, Lisbon (Portugal); INFN - sez. Torino (Italy); Silva, Jose C.; Varela, Joao [LIP, Lisbon (Portugal); PETsys Electronics, Oeiras (Portugal)

    2016-07-11

    We present a readout and digitization ASIC featuring low-noise and low-power for time-of flight (TOF) applications using SiPMs. The circuit is designed in standard CMOS 110 nm technology, has 64 independent channels and is optimized for time-of-flight measurement in Positron Emission Tomography (TOF-PET). The input amplifier is a low impedance current conveyor based on a regulated common-gate topology. Each channel has quad-buffered analogue interpolation TDCs (time binning 20 ps) and charge integration ADCs with linear response at full scale (1500 pC). The signal amplitude can also be derived from the measurement of time-over-threshold (ToT). Simulation results show that for a single photo-electron signal with charge 200 (550) fC generated by a SiPM with (320 pF) capacitance the circuit has 24 (30) dB SNR, 75 (39) ps r.m.s. resolution, and 4 (8) mW power consumption. The event rate is 600 kHz per channel, with up to 2 MHz dark counts rejection.

  5. Development of the STEFF detector for the neutron Time Of Flight facility (n_TOF), CERN

    CERN Document Server

    AUTHOR|(CDS)2092031

    Signicant work has been performed on the development of STEFF (SpecTrometer for Exotic Fission Fragments), a 2E2V (2-Energy 2-Velocity) spectrometer built by the University of Manchester Fission Group. The majority of this work was in the development of the time-of-flight systems, in particular the stop detector; with the main goals of improving the timing resolution and the detection eciency of the ssion fragments. Further development of the STEFF spectrometer was done to enable 2E2V measurements of the $^{235}$U(n,f) reaction with coincident measurements using a white neutron spectra of energies ranging from 10 meV to 200 MeV provided by the n_TOF (neutron Time Of Flight) facility, CERN. The STEFF spectrometer was successfully operated twice on the Experimental Area-2 high flux pulsed neutron beam line resulting in 2E2V measurements for ssion events with neutron energies ranging from 20 meV to 10 MeV. The first experiment received 1.36 X 10$^{18}$ POT (Protons On Target) with stable conditions and the seco...

  6. Laser desorption and time-of-flight mass spectrometry. Fundamentals .Applications

    International Nuclear Information System (INIS)

    Chaurand, P.

    1994-11-01

    Time-of-flight mass spectrometry is a very powerful technique for the analysis of heavy molecular ions (100 000 u and more). The ejection in the gas phase and the ionization of these molecules is now possible through the MALDI technique (Matrix Assisted Laser Desorption Ionization). This technique consists in mixing the heavy molecules to be analysed with a organic matrix which absorbs at the wavelength of the laser. The necessary irradiance are of the order of 10 6 W/cm 2 . In these conditions we have shown that the mass resolutions are optimum and that the relative mass accuracies are of the order of 10 -4 . We have also demonstrated that the emission angle of the molecular ions in MALDI depends on the incident angle of the laser light. During the desorption process, the molecular ions are emitted in the opposite direction of the incident laser light. This effect is particularly important for the design of the accelerating stage of the time-of-flight spectrometers. Problems relative to the detection of these heavy molecular ions have been studied in details between 0.5 10 4 m/s and 10 5 m/s. The velocity threshold of the electronic emission is lower than the value of 0.5 10 4 m/s. The relation between the electronic emission and the projectile velocity is complex. Finally, examples on mass identification of C 60 molecules and derivated C 60 are presented. Desorption methods are compared. (author). 32 refs., 34 figs

  7. Studying time of flight imaging through scattering media across multiple size scales (Conference Presentation)

    Science.gov (United States)

    Velten, Andreas

    2017-05-01

    Light scattering is a primary obstacle to optical imaging in a variety of different environments and across many size and time scales. Scattering complicates imaging on large scales when imaging through the atmosphere when imaging from airborne or space borne platforms, through marine fog, or through fog and dust in vehicle navigation, for example in self driving cars. On smaller scales, scattering is the major obstacle when imaging through human tissue in biomedical applications. Despite the large variety of participating materials and size scales, light transport in all these environments is usually described with very similar scattering models that are defined by the same small set of parameters, including scattering and absorption length and phase function. We attempt a study of scattering and methods of imaging through scattering across different scales and media, particularly with respect to the use of time of flight information. We can show that using time of flight, in addition to spatial information, provides distinct advantages in scattering environments. By performing a comparative study of scattering across scales and media, we are able to suggest scale models for scattering environments to aid lab research. We also can transfer knowledge and methodology between different fields.

  8. A fast large-area position-sensitive time-of-flight neutron detection system

    International Nuclear Information System (INIS)

    Crawford, R.K.; Haumann, J.R.

    1989-01-01

    A new position-sensitive time-of-flight neutron detection and histograming system has been developed for use at the Intense Pulsed Neutron Source. Spatial resolution of roughly 1 cm x 1 cm and time-of-flight resolution of ∼1 μsec are combined in a detection system which can ultimately be expanded to cover several square meters of active detector area. This system is based on the use of arrays of cylindrical one-dimensional position-sensitive proportional counters, and is capable of collecting the x-y-t data and sorting them into histograms at time-averaged data rates up to ∼300,000 events/sec over the full detector area and with instantaneous data rates up to more than fifty times that. Numerous hardware features have been incorporated to facilitate initial tuning of the position encoding, absolute calibration of the encoded positions, and automatic testing for drifts. 7 refs., 11 figs., 1 tabs

  9. Fast neutron measurements at the nELBE time-of-flight facility

    Directory of Open Access Journals (Sweden)

    Junghansa A. R.

    2015-01-01

    Full Text Available The compact neutron-time-of-flight facility nELBE at the superconducting electron accelerator ELBE of Helmholtz-Zentrum Dresden-Rossendorf has been rebuilt. A new enlarged experimental hall with a flight path of up to 10 m is available for neutron time-of-flight experiments in the fast energy range from about 50 keV to 10 MeV. nELBE is intended to deliver nuclear data of fast neutron nuclear interactions e.g. for the transmutation of nuclear waste and improvement of neutron physical simulations of innovative nuclear systems. The experimental programme consists of transmission measurements of neutron total cross sections, elastic and inelastic scattering cross section measurements, and neutron induced fission cross sections. The inelastic scattering to the first few excited states in 56Fe was investigated by measuring the gamma production cross section with an HPGe detector. The neutron induced fission of 242Pu was studied using fast ionisation chambers with large homogeneous actinide deposits.

  10. Neutron Spectroscopy for pulsed beams with frame overlap using a double time-of-flight technique

    Science.gov (United States)

    Harrig, K. P.; Goldblum, B. L.; Brown, J. A.; Bleuel, D. L.; Bernstein, L. A.; Bevins, J.; Harasty, M.; Laplace, T. A.; Matthews, E. F.

    2018-01-01

    A new double time-of-flight (dTOF) neutron spectroscopy technique has been developed for pulsed broad spectrum sources with a duty cycle that results in frame overlap, where fast neutrons from a given pulse overtake slower neutrons from previous pulses. Using a tunable beam at the 88-Inch Cyclotron at Lawrence Berkeley National Laboratory, neutrons were produced via thick-target breakup of 16 MeV deuterons on a beryllium target in the cyclotron vault. The breakup spectral shape was deduced from a dTOF measurement using an array of EJ-309 organic liquid scintillators. Simulation of the neutron detection efficiency of the scintillator array was performed using both GEANT4 and MCNP6. The efficiency-corrected spectral shape was normalized using a foil activation technique to obtain the energy-dependent flux of the neutron beam at zero degrees with respect to the incoming deuteron beam. The dTOF neutron spectrum was compared to spectra obtained using HEPROW and GRAVEL pulse height spectrum unfolding techniques. While the unfolding and dTOF results exhibit some discrepancies in shape, the integrated flux values agree within two standard deviations. This method obviates neutron time-of-flight spectroscopy challenges posed by pulsed beams with frame overlap and opens new opportunities for pulsed white neutron source facilities.

  11. Contribution of time-of-flight information to limited-angle positron tomography

    International Nuclear Information System (INIS)

    Macdonald, B.; Perez-Mendez, V.; Tam, K.C.

    1981-10-01

    Limited-angle emission tomography was investigated using a two-dimensional phantom to generate positron events simulating a camera with two opposed parallel position-sensitive detectors collecting data within a 90 0 cone. The data, backprojected onto lines passing through the phantom volume, is used with a matrix reconstruction method to provide two-dimensional images. Image quality was measured using the standard deviation of the reconstructions with respect to the original phantom. The application of Phillips-Twomey smoothing to the deconvolution matrices has substantially improved the original reconstructions, a factor of 1.9 in signal to noise ratio, giving S/N = 3.4 for a phantom having an average of 150 events/pixel. Using photon time-of-flight to restrict the reconstruction volume a further considerable improvement is made. When the time-of-flight limited the contributing volume to 4 lines out of 11 the improvement was another factor of 1.9 giving S/N = 6.0 for the same phantom. Comparable increases in signal to noise ratios are expected for three-dimensional reconstructions

  12. Laser ionization time of flight mass spectrometer for isotope mass detection and elemental analysis of materials

    Science.gov (United States)

    Ahmed, Nasar; Ahmed, Rizwan; Umar, Z. A.; Aslam Baig, M.

    2017-08-01

    In this paper we present the construction and modification of a linear time-of-flight mass spectrometer to improve its mass resolution. This system consists of a laser ablation/ionization section based on a Q-switched Nd:YAG laser (532 nm, 500 mJ, 5 ns pulse duration) integrated with a one meter linear time-of-flight mass spectrometer coupled with an electric sector and a magnetic lens and outfitted with a channeltron electron multiplier for ion detection. The resolution of the system has been improved by optimizing the accelerating potential and inserting a magnetic lens after the extraction region. The isotopes of lithium, lead and cadmium samples have been resolved and detected in accordance with their natural abundance. The capability of the system has been further exploited to determine the elemental composition of a brass alloy, having a certified composition of zinc and copper. Our results are in excellent agreement with its certified composition. This setup is found to be extremely efficient and convenient for fast analyses of any solid sample.

  13. TORCH: A Large-Area Detector for Precision Time-of-Flight Measurements at LHCb

    CERN Document Server

    Harnew, N

    2012-01-01

    The TORCH (Time Of internally Reflected CHerenkov light) is an innovative high-precision time-of-flight detector which is suitable for large areas, up to tens of square metres, and is being developed for the upgraded LHCb experiment. The TORCH provides a time-of-flight measurement from the imaging of photons emitted in a 1 cm thick quartz radiator, based on the Cherenkov principle. The photons propagate by total internal reflection to the edge of the quartz plane and are then focused onto an array of Micro-Channel Plate (MCP) photon detectors at the periphery of the detector. The goal is to achieve a timing resolution of 15 ps per particle over a flight distance of 10 m. This will allow particle identification in the challenging momentum region up to 20 GeV/c. Commercial MCPs have been tested in the laboratory and demonstrate the required timing precision. An electronics readout system based on the NINO and HPTDC chipset is being developed to evaluate an 8×8 channel TORCH prototype. The simulated performance...

  14. The multiple disk chopper neutron time-of-flight spectrometer at NIST

    International Nuclear Information System (INIS)

    Altorfer, F.B.; Cook, J.C.; Copley, J.R.D.

    1995-01-01

    A highly versatile multiple disk chopper neutron time-of-flight spectrometer is being installed at the Cold Neutron Research Facility of the National institute of Standards and Technology. This new instrument will fill an important gap in the portfolio of neutron inelastic scattering spectrometers in North America. It will be used for a wide variety of experiments such as studies of magnetic and vibrational excitations, tunneling spectroscopy, and quasielastic neutron scattering investigations of local and translational diffusion. The instrument uses disk choppers to monochromate and pulse the incident beam, and the energy changes of scattered neutrons are determined from their times-of-flight to a large array of detectors. The disks and the guide have been designed to make the instrument readily adaptable to the specific performance requirements of experimenters. The authors present important aspects of the design, as well as estimated values of the flux at the sample and the energy resolution for elastic scattering. The instrument should be operational in 1996

  15. Time-of-flight discrimination between gamma-rays and neutrons by using artificial neural networks

    International Nuclear Information System (INIS)

    Akkoyun, S.

    2013-01-01

    Highlights: ► Time-of-flight (tof) is an obvious method for separation between gamma and neutron particles. ► tof distributions are obtained by neural networks. ► Neural network method is consistent with the experimental results. ► Neural networks can classify different events for discrimination. - Abstract: In gamma-ray spectroscopy, a number of neutrons are emitted from the nuclei together with the gamma-rays. These neutrons influence gamma-ray spectra. An obvious method for discrimination between neutrons and gamma-rays is based on the time-of-flight (tof) technique. In this work, the tof distributions of gamma-rays and neutrons were obtained both experimentally and by using artificial neural networks (ANNs). It was shown that, ANN can correctly classify gamma-ray and neutron events. Also, for highly nonlinear detector response for tof, we have constructed consistent empirical physical formulas (EPFs) by appropriate ANNs. These ANN–EPFs can be used to derive further physical functions which could be relevant to discrimination between gamma-rays and neutrons

  16. Modeling of a 3D CMOS sensor for time-of-flight measurements

    Science.gov (United States)

    Kuhla, Rico; Hosticka, Bedrich J.; Mengel, Peter; Listl, Ludwig

    2004-02-01

    A solid state 3D-CMOS camera system for direct time-of-flight image acquisition consisting of a CMOS imaging sensor, a laser diode module for active laser pulse illumination and all optics for image forming is presented, including MDSI & CDS algorithms for time-of-flight evaluation from intensity imaging. The investigation is carried out using ideal and real signals. For real signals the narrow infrared laser pulse of the laser diode module and the shutter function of the sensors column circuit were sampled by a new sampling procedure. A discrete sampled shutter function was recorded by using the impulse response of a narrow pulse of FWHM=50ps and an additional delay block with step size of Δτ = 0.25ns. A deterministic system model based on LTI transfer functions was developed. The visual shutter windows give a good understanding of differences between ideal and real output functions of measurement system. Simulations of shutter and laser pulse brought out an extended linear delay domain from MDSI. A stochastic model for the transfer function and photon noise in time domain was developed. We used the model to investigate noise in variation the laser pulse shutter configuration.

  17. TOF plotter - a program to perform routine analysis time-of-flight mass spectral data

    International Nuclear Information System (INIS)

    Knippel, Brad C.; Padgett, Clifford W.; Marcus, R. Kenneth

    2004-01-01

    The main article discusses the operation and application of the program to mass spectral data files. This laboratory has recently reported the construction and characterization of a linear time-of-flight mass spectrometer (ToF-MS) utilizing a radio frequency glow discharge ionization source. Data acquisition and analysis was performed using a digital oscilloscope and Microsoft Excel, respectively. Presently, no software package is available that is specifically designed for time-of-flight mass spectral analysis that is not instrument dependent. While spreadsheet applications such as Excel offer tremendous utility, they can be cumbersome when repeatedly performing tasks which are too complex or too user intensive for macros to be viable. To address this situation and make data analysis a faster, simpler task, our laboratory has developed a Microsoft Windows-based software program coded in Microsoft Visual Basic. This program enables the user to rapidly perform routine data analysis tasks such as mass calibration, plotting and smoothing on x-y data sets. In addition to a suite of tools for data analysis, a number of calculators are built into the software to simplify routine calculations pertaining to linear ToF-MS. These include mass resolution, ion kinetic energy and single peak identification calculators. A detailed description of the software and its associated functions is presented followed by a characterization of its performance in the analysis of several representative ToF-MS spectra obtained from different GD-ToF-MS systems

  18. Satellite-borne time-of-flight particle spectrometer and its response to protons

    International Nuclear Information System (INIS)

    Shino, T.

    1994-01-01

    One of the purposes of the high energy particle (HEP) experiment of the GEOTAIL satellite launched in 1992 is the elucidation of plasma dynamics in the tail region of planetary magnetosphere. For that purpose, a low energy particle detector (LD) was on board, which mainly observed relatively low energy particles up to a few MeV. The LD is the particle spectrometer based on time of flight technique. In order to confirm further its sensitivity to high energy protons, the beam experiment was carried out at Waseda University using the engineering model of the LD spectrometer that is exactly the same as the launched one. The LD spectrometer is shown, and its functions are explained. The LD was designed to identify electrons of 30 - 400 keV, protons of 30 - 1500 keV, helium ions of 80 - 4000 keV, and heavy ions (mainly C, N and O) of 160 - 1500 keV. The relation of measured time of flight signals with energy signals is shown. There are several factors that determine the detection efficiency of the spectrometer, which are discussed. The experiment and the results are reported. (K.I.)

  19. Time-frequency energy density precipitation method for time-of-flight extraction of narrowband Lamb wave detection signals

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Y., E-mail: thuzhangyu@foxmail.com; Huang, S. L., E-mail: huangsling@tsinghua.edu.cn; Wang, S.; Zhao, W. [State Key Laboratory of Power Systems, Department of Electrical Engineering, Tsinghua University, Beijing 100084 (China)

    2016-05-15

    The time-of-flight of the Lamb wave provides an important basis for defect evaluation in metal plates and is the input signal for Lamb wave tomographic imaging. However, the time-of-flight can be difficult to acquire because of the Lamb wave dispersion characteristics. This work proposes a time-frequency energy density precipitation method to accurately extract the time-of-flight of narrowband Lamb wave detection signals in metal plates. In the proposed method, a discrete short-time Fourier transform is performed on the narrowband Lamb wave detection signals to obtain the corresponding discrete time-frequency energy density distribution. The energy density values at the center frequency for all discrete time points are then calculated by linear interpolation. Next, the time-domain energy density curve focused on that center frequency is precipitated by least squares fitting of the calculated energy density values. Finally, the peak times of the energy density curve obtained relative to the initial pulse signal are extracted as the time-of-flight for the narrowband Lamb wave detection signals. An experimental platform is established for time-of-flight extraction of narrowband Lamb wave detection signals, and sensitivity analysis of the proposed time-frequency energy density precipitation method is performed in terms of propagation distance, dispersion characteristics, center frequency, and plate thickness. For comparison, the widely used Hilbert–Huang transform method is also implemented for time-of-flight extraction. The results show that the time-frequency energy density precipitation method can accurately extract the time-of-flight with relative error of <1% and thus can act as a universal time-of-flight extraction method for narrowband Lamb wave detection signals.

  20. Time-frequency energy density precipitation method for time-of-flight extraction of narrowband Lamb wave detection signals

    International Nuclear Information System (INIS)

    Zhang, Y.; Huang, S. L.; Wang, S.; Zhao, W.

    2016-01-01

    The time-of-flight of the Lamb wave provides an important basis for defect evaluation in metal plates and is the input signal for Lamb wave tomographic imaging. However, the time-of-flight can be difficult to acquire because of the Lamb wave dispersion characteristics. This work proposes a time-frequency energy density precipitation method to accurately extract the time-of-flight of narrowband Lamb wave detection signals in metal plates. In the proposed method, a discrete short-time Fourier transform is performed on the narrowband Lamb wave detection signals to obtain the corresponding discrete time-frequency energy density distribution. The energy density values at the center frequency for all discrete time points are then calculated by linear interpolation. Next, the time-domain energy density curve focused on that center frequency is precipitated by least squares fitting of the calculated energy density values. Finally, the peak times of the energy density curve obtained relative to the initial pulse signal are extracted as the time-of-flight for the narrowband Lamb wave detection signals. An experimental platform is established for time-of-flight extraction of narrowband Lamb wave detection signals, and sensitivity analysis of the proposed time-frequency energy density precipitation method is performed in terms of propagation distance, dispersion characteristics, center frequency, and plate thickness. For comparison, the widely used Hilbert–Huang transform method is also implemented for time-of-flight extraction. The results show that the time-frequency energy density precipitation method can accurately extract the time-of-flight with relative error of <1% and thus can act as a universal time-of-flight extraction method for narrowband Lamb wave detection signals.

  1. COINTOF mass spectrometry: design of a time-of-flight analyzer and development of the analysis method

    International Nuclear Information System (INIS)

    Teyssier, C.

    2012-01-01

    DIAM (Device for the irradiation of molecular clusters) is a newly designed experimental setup to investigate processes resulting from the irradiation of molecular nano-systems by 20-150 keV protons. One of its specificities relies on the original technique of mass spectrometry named COINTOF (Correlated Ion and Neutral Time Of Flight) consisting in correlated measurements of the time of flight of charged and neutral fragments produced by the dissociation of a single molecular ion parent. A strategy of treatment and analysis of the detection signals was developed to distinguish two fragments close in time ( 3 O + and two water molecules. The distribution of the time of flight difference between the two neutral fragments is measured providing an estimate of the kinetic energy release of a few eV. In parallel, a second time-of-flight mass spectrometer was designed. It associates a linear time-of-flight and an orthogonal time-of-flight and integrates position detectors (delay line anode). Simulations demonstrate the potentials of the new analyzer. Finally, research works were led at the laboratory R.-J. A. Levesque (Universite de Montreal) on the imaging capabilities of the multi-pixel detectors of the MPX-ATLAS collaboration. (author)

  2. Development of grazing incidence devices for space-borne time of flight mass spectrometry

    Science.gov (United States)

    Cadu, A.; Devoto, P.; Louarn, P.; Sauvaud, J.-A.

    2012-04-01

    Time of flight mass spectrometer is widely used to study space plasmas in planetary and solar missions. This space-borne instrument selects ions in function of their energy through an electrostatic analyzer. Particles are then post-accelerated to energies in the range of 20 keV to cross a carbon foil. At the foil exit, electrons are emitted and separated from ion beam in the time of flight section. A first detector (a Micro-Channel Plate or MCP) emits a start signal at electron arrival and a second one emits a stop signal at incident ion end of path. The time difference gives the speed of the particle and its mass can be calculated, knowing its initial energy. However, current instruments suffer from strong limitations. The post acceleration needs very high voltage power supplies which are heavy, have a high power consumption and imply technical constraints for the development. A typical instrument weighs from 5 to 6 kg, includes a 20 kV power supply, consumes a least 5 W and encounters corona effect and electrical breakdown problems. Moreover, despite the particle high energy range, scattering and straggling phenomena in the carbon foil significantly reduce the instrument overall resolution. Some methods, such as electrostatic focus lenses or reflectrons, really improve mass separation but global system efficiency remains very low because of the charge state dependence of such devices. The main purpose of our work is to replace carbon foil by grazing incidence MCP's - also known as MPO's, for Micro Pore Optics - for electron emission. Thus, incident particles would back-scatter onto the channel inner surface with an angle of a few degrees. With this solution, we can decrease dispersion sources and lower the power supplies to post accelerate ions. The result would be a lighter and simpler instrument with a substantial resolution improvement. We have first simulated MPO's behavior with TRIM and MARLOWE Monte-Carlo codes. Energy scattering and output angle computed

  3. Quantitative myocardial blood flow imaging with integrated time-of-flight PET-MR.

    Science.gov (United States)

    Kero, Tanja; Nordström, Jonny; Harms, Hendrik J; Sörensen, Jens; Ahlström, Håkan; Lubberink, Mark

    2017-12-01

    The use of integrated PET-MR offers new opportunities for comprehensive assessment of cardiac morphology and function. However, little is known on the quantitative accuracy of cardiac PET imaging with integrated time-of-flight PET-MR. The aim of the present work was to validate the GE Signa PET-MR scanner for quantitative cardiac PET perfusion imaging. Eleven patients (nine male; mean age 59 years; range 46-74 years) with known or suspected coronary artery disease underwent 15 O-water PET scans at rest and during adenosine-induced hyperaemia on a GE Discovery ST PET-CT and a GE Signa PET-MR scanner. PET-MR images were reconstructed using settings recommended by the manufacturer, including time-of-flight (TOF). Data were analysed semi-automatically using Cardiac VUer software, resulting in both parametric myocardial blood flow (MBF) images and segment-based MBF values. Correlation and agreement between PET-CT-based and PET-MR-based MBF values for all three coronary artery territories were assessed using regression analysis and intra-class correlation coefficients (ICC). In addition to the cardiac PET-MR reconstruction protocol as recommended by the manufacturer, comparisons were made using a PET-CT resolution-matched reconstruction protocol both without and with TOF to assess the effect of time-of-flight and reconstruction parameters on quantitative MBF values. Stress MBF data from one patient was excluded due to movement during the PET-CT scanning. Mean MBF values at rest and stress were (0.92 ± 0.12) and (2.74 ± 1.37) mL/g/min for PET-CT and (0.90 ± 0.23) and (2.65 ± 1.15) mL/g/min for PET-MR (p = 0.33 and p = 0.74). ICC between PET-CT-based and PET-MR-based regional MBF was 0.98. Image quality was improved with PET-MR as compared to PET-CT. ICC between PET-MR-based regional MBF with and without TOF and using different filter and reconstruction settings was 1.00. PET-MR-based MBF values correlated well with PET-CT-based MBF values and

  4. A time-focusing Fourier chopper time-of-flight diffractometer for large scattering angles

    International Nuclear Information System (INIS)

    Heinonen, R.; Hiismaeki, P.; Piirto, A.; Poeyry, H.; Tiitta, A.

    1975-01-01

    A high-resolution time-of-flight diffractometer utilizing time focusing principles in conjunction with a Fourier chopper is under construction at Otaniemi. The design is an improved version of a test facility which has been used for single-crystal and powder diffraction studies with promising results. A polychromatic neutron beam from a radial beam tube of the FiR 1 reactor, collimated to dia. 70 mm, is modulated by a Fourier chopper (dia. 400 mm) which is placed inside a massive boron-loaded particle board shielding of 900 mm wall thickness. A thin flat sample (5 mm x dia. 80 mm typically) is mounted on a turntable at a distance of 4 m from the chopper, and the diffracted neutrons are counted by a scintillation detector at 4 m distance from the sample. The scattering angle 2theta can be chosen between 90deg and 160deg to cover Bragg angles from 45deg up to 80deg. The angle between the chopper disc and the incident beam direction as well as the angle of the detector surface relative to the diffracted beam can be adjusted between 45deg and 90deg in order to accomplish time-focusing. In our set-up, with equal flight paths from chopper to sample and from sample to detector, the time-focusing conditions are fulfilled when the chopper and the detector are parallel to the sample-plane. The time-of-flight spectrum of the scattered neutrons is measured by the reverse time-of-flight method in which, instead of neutrons, one essentially records the modulation function of the chopper during constant periods preceding each detected neutron. With a Fourier chopper whose speed is varied in a suitable way, the method is equivalent to the conventional Fourier method but the spectrum is obtained directly without any off-line calculations. The new diffractometer is operated automatically by a Super Nova computer which not only accumulates the synthetized diffraction pattern but also controls the chopper speed according to the modulation frequency sweep chosen by the user to obtain a

  5. Time-of-flight spectroscopy of metastable photodissociation fragments in vacuum-UV

    International Nuclear Information System (INIS)

    Fisher, C.H.; Welge, K.H.

    1974-01-01

    Photofragment time-of-flight experiments carried out at photon energies > approximately 11.8eV (1050A) is reported. Processes of the kind AB+hν→A*+B have been investigated where A* is an electronically excited species in a metastable state that can be detected by Auger electron emission from metal surfaces. The present work has been concerned with the identification of dissociation processes from N 2 O, CO 2 , and OCS, measurement of recoil energies and, for the first time, also angular dependent experiments. One objective of the work was to further explore the potential of such studies in the vacuum uv. Their feasibility was demonstrated previously in preliminary experiments

  6. Pose estimation and tracking of non-cooperative rocket bodies using Time-of-Flight cameras

    Science.gov (United States)

    Gómez Martínez, Harvey; Giorgi, Gabriele; Eissfeller, Bernd

    2017-10-01

    This paper presents a methodology for estimating the position and orientation of a rocket body in orbit - the target - undergoing a roto-translational motion, with respect to a chaser spacecraft, whose task is to match the target dynamics for a safe rendezvous. During the rendezvous maneuver the chaser employs a Time-of-Flight camera that acquires a point cloud of 3D coordinates mapping the sensed target surface. Once the system identifies the target, it initializes the chaser-to-target relative position and orientation. After initialization, a tracking procedure enables the system to sense the evolution of the target's pose between frames. The proposed algorithm is evaluated using simulated point clouds, generated with a CAD model of the Cosmos-3M upper stage and the PMD CamCube 3.0 camera specifications.

  7. Heavy ion time-of-flight ERDA of high dose metal implanted germanium

    Energy Technology Data Exchange (ETDEWEB)

    Dytlewski, N.; Evans, P.J.; Noorman, J.T. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia); Wielunski, L.S. [Commonwealth Scientific and Industrial Research Organisation (CSIRO), Lindfield, NSW (Australia). Div. of Applied Physics; Bunder, J. [New South Wales Univ., Wollongong, NSW (Australia). Wollongong Univ. Coll

    1996-12-31

    With the thick Ge substrates used in ion implantation, RBS can have difficulty in resolving the mass-depth ambiguities when analysing materials composed of mixtures of elements with nearly equal masses. Additional, and complimentary techniques are thus required. This paper reports the use of heavy ion time-of-flight elastic recoil detection analysis (ToF- ERDA), and conventional RBS in the analysis of Ge(100) implanted with high dose Ti and Cu ions from a MEWA ion source . Heavy ion ToF ERDA has been used to resolve, and profile the implanted transition metal species, and also to study any oxygen incorporation into the sample resulting from the implantation, or subsequential reactions with air or moisture. This work is part of a study on high dose metal ion implantation of medium atomic weight semiconductor materials. 13 refs., 6 figs.

  8. Stochastic calculus analysis of optical time-of-flight range imaging and estimation of radial motion.

    Science.gov (United States)

    Streeter, Lee

    2017-07-01

    Time-of-flight range imaging is analyzed using stochastic calculus. Through a series of interpretations and simplifications, the stochastic model leads to two methods for estimating linear radial velocity: maximum likelihood estimation on the transition probability distribution between measurements, and a new method based on analyzing the measured correlation waveform and its first derivative. The methods are tested in a simulated motion experiment from (-40)-(+40)  m/s, with data from a camera imaging an object on a translation stage. In tests maximum likelihood is slow and unreliable, but when it works it estimates the linear velocity with standard deviation of 1 m/s or better. In comparison the new method is fast and reliable but works in a reduced velocity range of (-20)-(+20)  m/s with standard deviation ranging from 3.5 m/s to 10 m/s.

  9. Heavy ion time-of-flight ERDA of high dose metal implanted germanium

    Energy Technology Data Exchange (ETDEWEB)

    Dytlewski, N; Evans, P J; Noorman, J T [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia); Wielunski, L S [Commonwealth Scientific and Industrial Research Organisation (CSIRO), Lindfield, NSW (Australia). Div. of Applied Physics; Bunder, J [New South Wales Univ., Wollongong, NSW (Australia). Wollongong Univ. Coll

    1997-12-31

    With the thick Ge substrates used in ion implantation, RBS can have difficulty in resolving the mass-depth ambiguities when analysing materials composed of mixtures of elements with nearly equal masses. Additional, and complimentary techniques are thus required. This paper reports the use of heavy ion time-of-flight elastic recoil detection analysis (ToF- ERDA), and conventional RBS in the analysis of Ge(100) implanted with high dose Ti and Cu ions from a MEWA ion source . Heavy ion ToF ERDA has been used to resolve, and profile the implanted transition metal species, and also to study any oxygen incorporation into the sample resulting from the implantation, or subsequential reactions with air or moisture. This work is part of a study on high dose metal ion implantation of medium atomic weight semiconductor materials. 13 refs., 6 figs.

  10. Fluence measurement at the neutron time of flight experiment at CERN

    CERN Document Server

    Weiss, Christina; Jericha, Erwin

    At the neutron time of flight facility n_TOF at CERN a new spallation target was installed in 2008. In 2008 and 2009 the commissioning of the new target took place. During the summer 2009 a fission chamber of the Physikalisch Technische Bundesanstalt (PTB) Braunschweig was used for the neutron fluence measurement. The evaluation of the data recorded with this detector is the primary topic of this thesis. Additionally a neutron transmission experiment with air has been performed at the TRIGA Mark II reactor of the Atomic Institute of the Austrian Universities (ATI). The experiment was implemented to clarify a question about the scattering cross section of molecular gas which could not be answered clearly via the literature. This problem came up during the evaluations for n_TOF.

  11. Ion-induced particle desorption in time-of-flight medium energy ion scattering

    Science.gov (United States)

    Lohmann, S.; Primetzhofer, D.

    2018-05-01

    Secondary ions emitted from solids upon ion impact are studied in a time-of-flight medium energy ion scattering (ToF-MEIS) set-up. In order to investigate characteristics of the emission processes and to evaluate the potential for surface and thin film analysis, experiments employing TiN and Al samples were conducted. The ejected ions exhibit a low initial kinetic energy of a few eV, thus, requiring a sufficiently high acceleration voltage for detection. Molecular and atomic ions of different charge states originating both from surface contaminations and the sample material are found, and relative yields of several species were determined. Experimental evidence that points towards a predominantly electronic sputtering process is presented. For emitted Ti target atoms an additional nuclear sputtering component is suggested.

  12. A time-of-flight spectrometer for neutron diffraction under high pressure or at high temperature

    International Nuclear Information System (INIS)

    Roult, G.; Buevoz, J.L.

    1975-01-01

    For high pressure neutron diffraction studies (40 kilobars) the sample is placed in a very thick cell. In order to allow the neutron beam to go through the cell loosing as little intensity as possible, the inner part is kept solid while the external part has some windows facing the incident and reflected beam. The window dimensions are small (a few millimeters wide and a few centimeters long). There are two alternatives: to have the window either in a perpendicular plane or in a plane parallel to the axis. In the first case a fixed wavelength spectrometer can be used but the sample is small and the contribution of the cell to the diffraction pattern is relatively great. In the second case samples can be something like ten times greater and the cell contribution can be eliminated but a fixed wavelength spectrometer cannot be used. Thus the time-of-flight method is very convenient. The second alternative was chosen

  13. Energy and time of flight measurements of REX-ISOLDE stable beams using Si detectors

    CERN Document Server

    Cantero, E D; Fraser, M A; Lanaia, D; Sosa, A; Voulot, D; Zocca, F

    2014-01-01

    In this paper we present energy and time spectroscopy measurements for the stable beams of REX-ISOLDE obtained using Si detectors. By using an alpha source as a calibration reference, the absolute energy E of stable beam particles (A/q = 4) was determined in spectroscopy mode in the energy range 1 MeV < E < 8 MeV (0.30 MeV/u < E/A < 1.87 MeV/u). The time of flight of the beam particles (2.18 MeV/u < E/A < 2.27 MeV/u) was determined by installing identical Si detectors in two diagnostic boxes separated by 7.7 m. The results obtained with these two techniques are compared with the values obtained by dipole scans using a bending magnet. The measurements took place between January and February of 2013.

  14. Time-of-flight neutron Bragg-edge transmission imaging of microstructures in bent steel plates

    Energy Technology Data Exchange (ETDEWEB)

    Su, Yuhua, E-mail: yuhua.su@j-parc.jp [J-PARC Center, Japan Atomic Energy Agency, 2-4 Shirakata, Tokai, Ibaraki 319-1195 (Japan); Oikawa, Kenichi; Harjo, Stefanus; Shinohara, Takenao; Kai, Tetsuya; Harada, Masahide; Hiroi, Kosuke [J-PARC Center, Japan Atomic Energy Agency, 2-4 Shirakata, Tokai, Ibaraki 319-1195 (Japan); Zhang, Shuoyuan; Parker, Joseph Don [Neutron R& D Division, CROSS-Tokai, 162-1 Shirakata, Tokai, Ibaraki 319-1106 (Japan); Sato, Hirotaka [Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Shiota, Yoshinori; Kiyanagi, Yoshiaki [Graduate School of Engineering, Nagoya University, Nagoya, Aichi 464-8603 (Japan); Tomota, Yo [Research Center for Strategic Materials, National Institute for Materials Science, Tsukuba 305-0047 (Japan)

    2016-10-15

    Neutron Bragg-edge transmission imaging makes it possible to quantitatively visualize the two-dimensional distribution of microstructure within a sample. In order to examine its application to engineering products, time-of-flight Bragg-edge transmission imaging experiments using a pulsed neutron source were performed for plastically bent plates composed of a ferritic steel and a duplex stainless steel. The non-homogeneous microstructure distributions, such as texture, crystalline size, phase volume fraction and residual elastic strain, were evaluated for the cross sections of the bent plates. The obtained results were compared with those by neutron diffraction and electron back scatter diffraction, showing that the Bragg-edge transmission imaging is powerful for engineering use.

  15. Development of time-of-flight RBS system using multi microchannel plates

    International Nuclear Information System (INIS)

    Nguyen, N.V.; Abo, S.; Lohner, T.; Sawaragi, H.; Wakaya, F.; Takai, M.

    2007-01-01

    A new time-of-flight Rutherford backscattering spectroscopy (TOF-RBS) system with two circular microchannel plates (MCPs) installed at a distance of 140 mm from a sample holder and a scattering angle of 125 o and a 100 kV focused ion beam column having a liquid metal ion source (LMIS) of AuSiBe alloy has been assembled to obtain high counting rate and enhanced mass resolution. The possible influence of the two MCPs by logical summation of the output signals on the time resolution was investigated by measuring dedicated thin deposited metallic samples. And, the time resolution was found in the range of 1.5-2 ns

  16. Laser Time-of-Flight Mass Spectrometry for Future In Situ Planetary Missions

    Science.gov (United States)

    Getty, S. A.; Brinckerhoff, W. B.; Cornish, T.; Ecelberger, S. A.; Li, X.; Floyd, M. A. Merrill; Chanover, N.; Uckert, K.; Voelz, D.; Xiao, X.; hide

    2012-01-01

    Laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) is a versatile, low-complexity instrument class that holds significant promise for future landed in situ planetary missions that emphasize compositional analysis of surface materials. Here we describe a 5kg-class instrument that is capable of detecting and analyzing a variety of analytes directly from rock or ice samples. Through laboratory studies of a suite of representative samples, we show that detection and analysis of key mineral composition, small organics, and particularly, higher molecular weight organics are well suited to this instrument design. A mass range exceeding 100,000 Da has recently been demonstrated. We describe recent efforts in instrument prototype development and future directions that will enhance our analytical capabilities targeting organic mixtures on primitive and icy bodies. We present results on a series of standards, simulated mixtures, and meteoritic samples.

  17. System architecture for high speed reconstruction in time-of-flight positron tomography

    International Nuclear Information System (INIS)

    Campagnolo, R.E.; Bouvier, A.; Chabanas, L.; Robert, C.

    1985-06-01

    A new generation of Time Of Flight (TOF) positron tomograph with high resolution and high count rate capabilities is under development in our group. After a short recall of the data acquisition process and image reconstruction in a TOF PET camera, we present the data acquisition system which achieves a data transfer rate of 0.8 mega events per second or more if necessary in list mode. We describe the reconstruction process based on a five stages pipe line architecture using home made processors. The expected performance with this architecture is a time reconstruction of six seconds per image (256x256 pixels) of one million events. This time could be reduce to 4 seconds. We conclude with the future developments of the system

  18. Monte Carlo study of the performance of a time-of-flight multichopper spectrometer

    International Nuclear Information System (INIS)

    Daemen, L.L.; Eckert, J.; Pynn, R.

    1995-01-01

    The Monte Carlo method is a powerful technique for neutron transport studies. While it has been applied for many years to the study of nuclear systems, there are few codes available for neutron transport in the optical regime. The recent surge of interest in so-called next generation spallation neutron sources and the desire to design new and optimized instruments for these facilities has led us to develop a Monte Carlo code geared toward the simulation of neutron scattering instruments. The time-of-flight multichopper spectrometer, of which IN5 at the ILL is the prototypical example, is the first spectrometer studied with the code. Some of the results of a comparison between the IN5 performance at a reactor and at a Long Pulse Spallation Source (LPSS) are summarized here

  19. Low-pressure, multistep, multiwire proportional counter for the time-of-flight isochronous spectrometer

    International Nuclear Information System (INIS)

    Vieira, D.J.

    1985-01-01

    A low-pressure, multistep, multiwire proportional counter (MSMWPC) has been developed for the characterization and testing of the time-of-flight isochronous (TOFI) spectrometer and its associated secondary-beam transport line. This type of counter was selected because of its high sensitivity, large dynamic range, and good position (0.2 mm FWHM) and timing (180 ps FWHM) resolution. Furthermore, because the counter operates at low gas pressures (1-10 torr) and high electric-field strengths, which enable short collection times, it can be used as a transmission counter with thin gas-isolation windows and it can operate at high counting rates. Here the authors discuss the basic operating principle of the MSMWPC, describe the technical details of the detector and signal processing, and report on the performance they have measured for alpha particles and fission fragments

  20. Ion optics of a new time-of-flight mass spectrometer for quantitative surface analysis

    International Nuclear Information System (INIS)

    Veryovkin, Igor V.; Calaway, Wallis F.; Pellin, Michael J.

    2004-01-01

    A new time-of-flight instrument for quantitative surface analysis was developed and constructed at Argonne National Laboratory. It implements ion sputtering and laser desorption for probing analyzed samples and can operate in regimes of secondary neutral mass spectrometry with laser post-ionization and secondary ion mass spectrometry. The instrument incorporates two new ion optics developments: (1) 'push-pull' front end ion optics and (2) focusing and deflecting lens. Implementing these novel elements significantly enhance analytical capabilities of the instrument. Extensive three-dimensional computer simulations of the instrument were conducted in SIMION 3D (c) to perfect its ion optics. The operating principles of the new ion optical systems are described, and a scheme of the new instrument is outlined together with its operating modes