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Sample records for gas chromatography ion-trap

  1. APPLICATION OF GC/ITD (GAS CHROMATOGRAPHY/ION TRAP DETECTOR) TO ENVIRONMENTAL ANALYSIS (JOURNAL VERSION)

    EPA Science Inventory

    The choice of gas chromatography (GC) detectors has expanded rapidly. The necessity for mass spectrometric (MS) characterization of GC effluents stems from the complexity of the matrices associated with environmental samples. There are currently several MS types being used in con...

  2. Gas chromatography-ion trap tandem mass spectrometry method for the analysis of methoxylated polybrominated diphenyl ethers in fish.

    PubMed

    Losada, S; Santos, F J; Covaci, A; Galceran, M T

    2010-08-01

    Gas chromatography coupled to ion trap tandem mass spectrometry (GC-ITMS-MS) is proposed for the analysis of methoxylated polybrominated diphenyl ethers (MeO-PBDEs) in fish and shellfish. MS-MS operating parameters related to the isolation and fragmentation of the precursor ions were optimized to achieve maximum sensitivity and selectivity. This new method allows the determination of both MeO-PBDEs and PBDEs in a single run. Low limits of detection (0.4-2.5 pg injected) and high precision (RSD<13%) were achieved. A sample treatment based on a selective pressurized liquid extraction (PLE) using Florisil as fat retainer was applied for the analysis of these compounds in fish samples. Method limits of quantification ranged from 0.11 to 0.95 ng g(-1) lipid weight for MeO-PBDEs and between 0.18 and 0.50 ng g(-1) lipid weight for PBDEs. In addition, good repeatability of the whole method was achieved (RSD<15%). The suitability of the method was evaluated by analyzing a certified reference material (SRM 1945, whale blubber) with satisfactory results. The developed method was applied to the simultaneous analysis of MeO-PBDEs and PBDEs in fish and shellfish samples from the Mediterranean Sea. PMID:20615508

  3. DETERMINATION OF INTERFERING TRIAZINE DEGRADATION PRODUCTS BY GAS CHROMATOGRAPHY-ION TRAP MASS SPECTROMETRY

    EPA Science Inventory

    Deethyl atrazine (DEA), along with other triazine degradation products, has been added to the US Environmental Protection Agency's Drinking Water Contaminant Candidate List (CCL). In its gas chromatographic (GC) analysis, deethyl atrazine, a degradation product of atrazine, can ...

  4. Miniaturized GC/MS instrumentation for in situ measurements: micro gas chromatography coupled with miniature quadrupole array and paul ion trap mass spectrometers

    NASA Technical Reports Server (NTRS)

    Holland, P.; Chutjian, A.; Darrach, M.; Orient, O.

    2002-01-01

    Miniaturized chemical instrumentation is needed for in situ measurements in planetary exploration and other spaceflight applications where factors such as reduction in payload requirements and enhanced robustness are important. In response to this need, we are 'continuing to develop miniaturized GC/MS instrumentation which combines chemical separations by gas chromatography (GC) with mass spectrometry (MS) to provide positive identification of chemical compounds in complex mixtures of gases, such as those found in the International Space Station's cabin atmosphere. Our design approach utilizes micro gas chromatography components coupled with either a miniature quadrupole mass spectrometer array (QMSA) or compact, high-resolution Paul ion trap.

  5. Characterization of the synthesis of N,N-dimethyltryptamine by reductive amination using gas chromatography ion trap mass spectrometry.

    PubMed

    Brandt, Simon D; Moore, Sharon A; Freeman, Sally; Kanu, Abu B

    2010-07-01

    The present study established an impurity profile of a synthetic route to the hallucinogenic N,N-dimethyltryptamine (DMT). The synthesis was carried out under reductive amination conditions between tryptamine and aqueous formaldehyde in the presence of acetic acid followed by reduction with sodium cyanoborohydride. Analytical characterization of this synthetic route was carried out by gas chromatography ion trap mass spectrometry using electron- and chemical-ionization modes. Methanol was employed as a liquid CI reagent and the impact of stoichiometric modifications on side-products formation was also investigated. Tryptamine 1, DMT 2, 2-methyltetrahydro-β-carboline (2-Me-THBC, 3), N-methyl-N-cyanomethyltryptamine (MCMT, 4), N-methyltryptamine (NMT, 5), 2-cyanomethyl-tetrahydro-β-carboline (2-CM-THBC, 6) and tetrahydro-β-carboline (THBC, 7) have been detected under a variety of conditions. Replacement of formaldehyde solution with paraformaldehyde resulted in incomplete conversion of the starting material whereas a similar replacement of sodium cyanoborohydride with sodium borohydride almost exclusively produced THBC instead of the expected DMT. Compounds 1 to 7 were quantified and the limits of detection were 28.4, 87.7, 21.5, 23.4, 41.1, 36.6, and 34.9 ng mL(-1), respectively. The limits of quantification for compounds 1 to 7 were 32.4, 88.3, 25.4, 24.6, 41.4, 39.9, and 37.0 µg mL(-1), respectively. Linearity was observed in the range of 20.8-980 µg mL(-1) with correlation coefficients > 0.99. The application holds great promise in the area of forensic chemistry where development of reliable analytical methods for the detection, identification, and quantification of DMT are crucial and also in pharmaceutical analysis where DMT might be prepared for use in human clinical studies. PMID:20648523

  6. Mass Spectrometry Parameters Optimization for the 46 Multiclass Pesticides Determination in Strawberries with Gas Chromatography Ion-Trap Tandem Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Fernandes, Virgínia C.; Vera, Jose L.; Domingues, Valentina F.; Silva, Luís M. S.; Mateus, Nuno; Delerue-Matos, Cristina

    2012-12-01

    Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or " q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.

  7. Method for Detection of Trace Metal and Metalloid Contaminants in Coal-Generated Fuel Gas Using Gas Chromatography/Ion Trap Mass Spectrometry

    SciTech Connect

    Rupp, Erik C.; Granite, Evan J.; Stanko, Dennis C.

    2010-07-15

    There exists an increasing need to develop a reliable method to detect trace contaminants in fuel gas derived from coal gasification. While Hg is subject to current and future regulations, As, Se, and P emissions may eventually be regulated. Sorbents are the most promising technology for the removal of contaminants from coal-derived fuel gas, and it will be important to develop a rapid analytical detection method to ensure complete removal and determine the ideal time for sorbent replacement/regeneration in order to reduce costs. This technical note explores the use of a commercial gas chromatography/ion trap mass spectrometry system for the detection of four gaseous trace contaminants in a simulated fuel gas. Quantitative, repeatable detection with limits at ppbv to ppmv levels were obtained for arsine (AsH3), phosphine (PH3), and hydrogen selenide (H2Se), while qualitative detection was observed for mercury. Decreased accuracy and response caused by the primary components of fuel gas were observed.

  8. Trace analysis of explosives in seawater using solid-phase microextraction and gas chromatography/ion trap mass spectrometry

    SciTech Connect

    Barshick, S.A.; Griest, W.H.

    1998-07-15

    Complex matrices typically cannot be analyzed directly to obtain the selectivity and sensitivity required for most trace analysis applications. To circumvent this problem, solid-phase microextraction (SPME) techniques were used to preconcentrate analytes selectively prior to gas chromatographic/ion trap mass spectrometric analysis. This approach was applied to the trace analysis of explosives and their metabolites in seawater. The choice of SPME sorbent phase was shown to be important especially for the amino metabolites of trinitrotoluene (TNT) and RDX, which were extracted better on polar phases. Although equilibration times were quite lengthy, on the order of 30 min or greater, a sampling time of only 10 min was shown to be sufficient for achieving low part-per-billion (ppb) to part-per-trillion (ppt) detection limits for TNT and the amino metabolites in real seawater samples. While SPME was ideal for rapid screening of explosives in seawater samples, methods for improving the reproducibility and accuracy of quantification are still being investigated.

  9. A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

    PubMed

    Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

    2003-01-01

    A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated. PMID:12587679

  10. Development and validation of automatic HS-SPME with a gas chromatography-ion trap/mass spectrometry method for analysis of volatiles in wines.

    PubMed

    Paula Barros, Elisabete; Moreira, Nathalie; Elias Pereira, Giuliano; Leite, Selma Gomes Ferreira; Moraes Rezende, Claudia; Guedes de Pinho, Paula

    2012-11-15

    An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed in order to quantify a large number of volatile compounds in wines such as alcohols, ester, norisoprenoids and terpenes. The procedures were optimized for SPME fiber selection, pre-incubation temperature and time, extraction temperature and time, and salt addition. A central composite experimental design was used in the optimization of the extraction conditions. The volatile compounds showed optimal extraction using a DVB/CAR/PDMS fiber, incubation of 5 ml of wine with 2g NaCl at 45 °C during 5 min, and subsequent extraction of 30 min at the same temperature. The method allowed the identification of 64 volatile compounds. Afterwards, the method was validated successfully for the most significant compounds and was applied to study the volatile composition of different white wines. PMID:23158309

  11. Volatile composition of Brassica oleracea L. var. costata DC leaves using solid-phase microextraction and gas chromatography/ion trap mass spectrometry.

    PubMed

    de Pinho, Paula Guedes; Valentão, Patrícia; Gonçalves, Rui F; Sousa, Carla; Andrade, Paula B

    2009-08-01

    Volatile and semi-volatile components of internal and external leaves of Brassica oleracea L. var. costata DC, grown under different fertilization regimens, were determined by headspace solid-phase microextraction (HS-SPME) combined with gas chromatography/ion trap mass spectrometry (GC/ITMS). Forty-one volatiles and non-volatile components were formally identified and thirty others were tentatively identified. Qualitative and quantitative differences were noticed between internal and external leaves. In general, internal leaves exhibited more aldehydes and sulfur volatile compounds than external ones, and less ketone, terpenes and norisoprenoid compounds. The fertilization regimens influenced considerably the volatile profile. Fertilizations with higher levels of sulfur produced Brassica leaves with more sulfur volatiles. In opposition, N and S fertilization led to leaves with lower levels of norisoprenoids and terpenes. PMID:19579264

  12. Analysis of the diastereoisomers of the cysteinylated aroma precursor of 3-sulfanylhexanol in Vitis vinifera grape must by gas chromatography coupled with ion trap tandem mass spectrometry.

    PubMed

    Thibon, Cécile; Shinkaruk, Svitlana; Tominaga, Takatoshi; Bennetau, Bernard; Dubourdieu, Denis

    2008-03-01

    The diastereoisomeric distribution of S-3-(hexan-1-ol)cysteine (P-3SH), the cysteinylated precursor of 3-sulfanylhexan-1-ol (3SH) in Vitis vinifera grape juice, was determined by a new method. This procedure is based on the purification of P-3SH in a small volume of must (500 microL) by affinity chromatography, followed by the separation of chiral molecules in derivative forms by gas chromatography coupled with ion trap tandem mass spectrometry (GC-MS/MS). The diastereoisomers were easily separated using heptafluorobutyric anhydride and heptafluorobutanol (HFBA and HFOH) as derivatization reagents. Method validation was conducted using samples of grape juice, synthetic must, fermenting must, and wine that were fortified with P-3SH at concentrations of 0.6 and 2.5 microM. The relative standard deviation (RSD) and limit of detection (LOD) of the GC-MS/MS method were 4.6% and 1.5 nM, respectively. P-3SH assays in Bordeaux white grape juice affected by Botrytis cinerea showed an unusually increased proportion of the RS form of the precursor (approximately RR:RS=30:70) as compared to a diastereoisomer ratio (in the vicinity of 50:50) in healthy grape juice. PMID:18249409

  13. Characterization of diacylglycerol isomers in edible oils using gas chromatography-ion trap electron ionization mass spectrometry.

    PubMed

    Zhu, Hanjiang; Clegg, Michael S; Shoemaker, Charles F; Wang, Selina C

    2013-08-23

    Verifying the authenticity of edible oils is of international concern. A new quality control standard for olive oil has been proposed that relates the ratio of 1,2-diacylglycerol (DAG) to 1,3-DAG to sensory aspects of olive oil. DAGs and their isomers are difficult to quantitate and characterize by Flame Ionization Gas Chromatography (GC-FID) due to the lack of suitable standards. Mass detectors offer the advantage of providing structural detail to the eluding DAG(s), thus removing ambiguity to the identification of both resolved and unresolved DAGs in GC chromatograms. In this study, a GC Electron Ionization Mass Spectrometry (GC-EI-MS) method was developed to determine the fatty acid composition and molecular structure of trimethylsilyl (TMS) derivatized DAGs present in edible oils. Twenty-two species of DAG isomers were identified in refined coconut oil and unrefined olive oil utilizing signature fragment ions, [M-15](+), [M-89](+), [M-RCO2](+), [RCO2+58](+) and [M-RCO2CH2](+). The [M-RCO2CH2](+) ion is considered the key diagnostic ion to distinguish between DAG positional isomers. MS/MS spectra of [M-RCO2](+) and [M-15](+) ions obtained from commercial standards containing both 1,2- and 1,3-DAG isomers were used as a model system to confirm the identification of DAG isomers in natural products. Furthermore, a number of reaction mechanisms are proposed to explain the formation of the most abundant mass fragments of DAGs and their isomers. PMID:23880469

  14. Determination of trace levels of herbicides and their degradation products in surface and ground waters by gas chromatography/ion-trap mass spectrometry

    USGS Publications Warehouse

    Pereira, W.E.; Rostad, C.E.; Leiker, T.J.

    1990-01-01

    A rapid, specific and highly sensitive method is described for the determination of several commonly used herbicides and their degradation products in surface and ground waters by using gas chromatography/ion-trap mass spectrometry. The compounds included atrazine, and its degradation products desethylatrazine and desisopropylatrazine; Simazine; Cyanazine; Metolachlor; and alachlor and its degradation products, 2-chloro-2', 6'-diethylacetanilide, 2-hydroxy-2', 6'-diethylacetanilide and 2,6-diethylaniline. The method was applied to surface-water samples collected from 16 different stations along the lower Mississippi River and its major tributaries, and ground-water samples beneath a cornfield in central Nebraska. Average recovery of a surrogate herbicide, terbuthylazine, was greater than 99%. Recoveries of the compounds of interest from river water spiked at environmental levels are also presented. Full-scan mass spectra of these compounds were obtained on 1 ng or less of analyte. Data were collected in the full-scan acquisition mode. Quantitation was based on a single characteristic ion for each compound. The detection limit was 60 pg with a signal-to-noise ratio of greater than 10:1.

  15. Determination of pesticides associated with suspended sediments in the San Joaquin River, California, USA, using gas chromatography-ion trap mass spectrometry

    USGS Publications Warehouse

    Bergamaschi, B.A.; Baston, D.S.; Crepeau, K.L.; Kuivila, K.M.

    1999-01-01

    An analytical method useful for the quantification of a range of pesticides and pesticide degradation products associated with suspended sediments was developed by testing a variety of extraction and cleanup schemes. The final extraction and cleanup methods chosen for use are suitable for the quantification of the listed pesticides using gas chromatography-ion trap mass spectrometry and the removal of interfering coextractable organic material found in suspended sediments. Methylene chloride extraction followed by Florisil cleanup proved most effective for separation of coextractives from the pesticide analytes. Removal of elemental sulfur was accomplished with tetrabutylammonium hydrogen sulfite. The suitability of the method for the analysis of a variety of pesticides was evaluated, and the method detection limits (MDLs) were determined (0.1-6.0 ng/g dry weight of sediment) for 21 compounds. Recovery of pesticides dried onto natural sediments averaged 63%. Analysis of duplicate San Joaquin River suspended-sediment samples demonstrated the utility of the method for environmental samples with variability between replicate analyses lower than between environmental samples. Eight of 21 pesticides measured were observed at concentrations ranging from the MDL to more than 80 ng/g dry weight of sediment and exhibited significant temporal variability. Sediment-associated pesticides, therefore, may contribute to the transport of pesticides through aquatic systems and should be studied separately from dissolved pesticides.

  16. Solid-phase microextraction gas chromatography/ion trap mass spectrometry and multistage mass spectrometry experiments in the characterization of germacrene D.

    PubMed

    Gioacchini, A M; Menotta, M; Polidori, E; Giomaro, G; Stocchi, V

    2002-12-01

    Germacrene D is a vegetable pheromone utilized in interactions among organisms belonging to different species. For the first time, using solid-phase microextraction/gas chromatography/ion trap mass spectrometry, the presence of this compound was detected in an in vitro mycorrhizal synthesis system where the mycelium of the ectomycorrhizal fungus Tuber borchii Vittad. interacts with the plant Tilia Americana L. From this symbiosis, a new structure, called ectomycorrhiza, is formed where the two symbionts exchange nutrients and metabolites. It seems that only after this interaction can the mycelium develop the fruitbody, commonly known as truffle. The results obtained allowed us to ascertain that germacrene D was synthesized by the plant exclusively in the presence of T. borchii. The originality of these data prompted us to hypothesize that this compound could be involved in the first step of ectomycorrhiza formation, as it is able to stimulate specific fungi receptors. In fact, plants release hundreds of secondary metabolites that are important in their interactions with other organisms. PMID:12489082

  17. Rapid and sensitive gas chromatography-ion-trap tandem mass spectrometry method for the determination of tobacco-specific N-nitrosamines in secondhand smoke.

    PubMed

    Sleiman, Mohamad; Maddalena, Randy L; Gundel, Lara A; Destaillats, Hugo

    2009-11-01

    Tobacco-specific nitrosamines (TSNAs) are some of the most potent carcinogens in tobacco and cigarette smoke. Accurate quantification of these chemicals is needed to help assess public health risks. We developed and validated a specific and sensitive method to measure four TSNAs adsorbed to model surfaces and secondhand smoke (SHS) particles using gas chromatography-ion-trap tandem mass spectrometry. In an 18-m(3) room-sized chamber, a smoking machine generated realistic concentrations of SHS that were actively sampled on Teflon-coated fiber glass (TCFG) filters, and passively sampled on cellulose substrates. A simple solid-liquid extraction protocol using methanol as solvent was successfully applied to both substrates with recoveries ranging from 85 to 115%. For each TSNA, tandem MS parameters were optimized and the major fragmentation pathways were elucidated. The method showed excellent performance, with a linear dynamic range from 2 to 1000ngmL(-1), low detection limits (S/N>3) of 30-300pgmL(-1) and precision with experimental errors below 10% for all compounds. Moreover, no interfering peaks were observed, indicating a high selectivity of MS/MS without the need for a sample clean-up step. This method provides a suitable analytical tool to detect and quantify traces of TSNA in indoor environments polluted with SHS. PMID:19800070

  18. Analysis of permethrin isomers in composite diet samples by molecularly imprinted solid-phase extraction and isotope dilution gas chromatography-ion trap mass spectrometry.

    PubMed

    Vonderheide, Anne P; Boyd, Brian; Ryberg, Anna; Yilmaz, Ecevit; Hieber, Thomas E; Kauffman, Peter E; Garris, Sherry T; Morgan, Jeffrey N

    2009-05-29

    Determination of an individual's aggregate dietary ingestion of pesticides entails analysis of a difficult sample matrix. Permethrin-specific molecularly imprinted polymer (MIP) solid-phase extraction cartridges were developed for use as a sample preparation technique for a composite food matrix. Vortexing with acetonitrile and centrifugation were found to provide optimal extraction of the permethrin isomers from the composite foods. The acetonitrile (with 1% acetic acid) was mostly evaporated and the analytes reconstituted in 90:10 water/acetonitrile in preparation for molecularly imprinted solid-phase extraction. Permethrin elution was accomplished with acetonitrile and sample extracts were analyzed by isotope dilution gas chromatography-ion trap mass spectrometry. Quantitation of product ions provided definitive identification of the pesticide isomers. The final method parameters were tested with fortified composite food samples of varying fat content (1%, 5%, and 10%) and recoveries ranged from 99.3% to 126%. Vegetable samples with incurred pesticide levels were also analyzed with the given method and recoveries were acceptable (81.0-95.7%). Method detection limits were demonstrated in the low ppb range. Finally, the applicability of the MIP stationary phase to extract other pyrethroids, specifically cyfluthrin and cypermethrin, was also investigated. PMID:19393156

  19. Rapid and sensitive gas chromatography ion-trap mass spectrometry method for the determination of tobacco specific N-nitrosamines in secondhand smoke

    SciTech Connect

    SLEIMAN, Mohamad; MADDALENA, Randy L.; GUNDEL, Lara A.; DESTAILLATS, Hugo

    2009-07-01

    Tobacco-specific nitrosamines (TSNAs) are some of the most potent carcinogens in tobacco and cigarette smoke. Accurate quantification of these chemicals is needed to help assess public health risks. We developed and validated a specific and sensitive method to measure four TSNAs in both the gas- and particle-phase of secondhand smoke (SHS) using gas chromatography and ion-trap tandem mass spectrometry,. A smoking machine in an 18-m3 room-sized chamber generated relevant concentrations of SHS that were actively sampled on Teflon coated fiber glass (TCFG) filters, and passively sampled on cellulose substrates. A simple solid-liquid extraction protocol using methanol as solvent was successfully applied to both filters with high recoveries ranging from 85 to 115percent. Tandem MS parameters were optimized to obtain the best sensitivity in terms of signal to-noise ratio (S/N) for the target compounds. For each TSNA, the major fragmentation pathways as well as ion structures were elucidated and compared with previously published data. The method showed excellent performances with a linear dynamic range between 2 and 1000 ng mL-1, low detection limits (S/N> 3) of 30-300 pg.ml-1 and precision with experimental errors below 10percent for all compounds. Moreover, no interfering peaks were observed indicating a high selectivity of MS/MS without the need for a sample clean up step. The sampling and analysis method provides a sensitive and accurate tool to detect and quantify traces of TSNA in SHS polluted indoor environments.

  20. Determination of N,N-dimethyltryptamine in beverages consumed in religious practices by headspace solid-phase microextraction followed by gas chromatography ion trap mass spectrometry.

    PubMed

    Gaujac, Alain; Dempster, Nicola; Navickiene, Sandro; Brandt, Simon D; de Andrade, Jailson Bittencourt

    2013-03-15

    A novel analytical approach combining solid-phase microextraction (SPME)/gas chromatography ion trap mass spectrometry (GC-IT-MS) was developed for the detection and quantification N,N-dimethyltryptamine (DMT), a powerful psychoactive indole alkaloid present in a variety of South American indigenous beverages, such as ayahuasca and vinho da jurema. These particular plant products, often used within a religious context, are increasingly consumed throughout the world following an expansion of religious groups and the availability of plant material over the Internet and high street shops. The method described in the present study included the use of SPME in headspace mode combined GC-IT-MS and included the optimization of the SPME procedure using multivariate techniques. The method was performed with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in headspace mode (70 min at 60 °C) which resulted in good precision (RSD<8.6%) and accuracy values (71-109%). Detection and quantification limits obtained for DMT were 0.78 and 9.5 mg L(-1), respectively and good linearity (1.56-300 mg L(-1), r(2)=0.9975) was also observed. In addition, the proposed method showed good robustness and allowed for the minimization of sample manipulation. Five jurema beverage samples were prepared in the laboratory in order to study the impact of temperature, pH and ethanol on the ability to extract DMT into solution. The developed method was then applied to the analysis of twelve real ayahuasca and vinho da jurema samples, obtained from Brazilian religious groups, which revealed DMT concentration levels between 0.10 and 1.81 g L(-1). PMID:23598143

  1. Determination of cis-permethrin, trans-permethrin and associated metabolites in rat blood and organs by gas chromatography-ion trap mass spectrometry.

    PubMed

    Lestremau, F; Willemin, M-E; Chatellier, C; Desmots, S; Brochot, C

    2014-05-01

    An analytical method was developed to measure cis-permethrin and trans-permethrin in different biological rat matrices and fluids (whole blood, red blood cells, plasma, brain, liver, muscle, testes, kidneys, fat and faeces). The method was also suitable for the simultaneous quantification of their associated metabolites [cis-3-(2,2-dichlorovinyl)-2,2-dimethyl-(1-cyclopropane) carboxylic acid (cis-DCCA), trans-3-(2,2-dichlorovinyl)-2,2-dimethyl-(1-cyclopropane) carboxylic acid (trans-DCCA) and 3-phenoxybenzoic acid (3-PBA)] in blood (whole blood, red blood cells, plasma) and liver. The target analytes were derivatised in samples using a methanolic/hydrochloric acid solution and then extracted with toluene. The analysis was performed by gas chromatography, and detection using ion trap tandem mass spectrometry. The selectivity obtained for complex matrices such as rat organs allowed the use of a purification step to be avoided for most of the matrices investigated. In the case of fat, where permethrin is suspected to accumulate, a dedicated purification step was developed. In fluids, the limits of quantification were at the 50 ng/mL level for the parent compounds and 3-PBA and at 25 ng/mL for cis-DCCA and trans-DCCA. For solid matrices excluding fat, the limits of quantification ranged from 50 ng/g for muscle to 100 ng/g for brain and testes for both cis-permethrin and trans-permethrin. The extraction recoveries ranged primarily between 80 and 120% for the matrix tested. The stability of blood samples was tested through the addition of 1% v/v formic acid. The methods developed were applied in a toxicokinetic study in adult rats. cis-Permethrin and the metabolites were detected in all corresponding matrices, whereas trans-permethrin was detected only in blood, plasma and faeces. PMID:24718437

  2. Determination of 23 pesticide residues in leafy vegetables using gas chromatography-ion trap mass spectrometry and analyte protectants.

    PubMed

    González-Rodríguez, Rosa Ma; Rial-Otero, Raquel; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2008-07-01

    A gas chromatographic method was developed for simultaneously determining residues of 12 insecticides (acrinathrin, bifenthrin, carbofuran, cyfluthrin, lambda-cyhalothrin, cypermethrin, chlorfenvinphos, deltamethrin, esfenvalerate, fenamiphos, methiocarb and tau-fluvalinate) and 11 fungicides (cyprodinil, fludioxonil, iprodione, metalaxyl, penconazole, pyrimethanil, procymidone tebuconazole, triadimefon, triadimenol and vinclozolin) in leafy vegetables. Samples were extracted with acetonitrile and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The eluate was finally evaporated and redissolved with 0.5 mL of acetone containing the internal standards (pentachlorobenzene and fenpropathrin) and three analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid gamma-lactone). The addition of analyte protectants allows to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 10% for all pesticides and finally, limits of detection were also 10-20 times lower than maxima residue levels (MRLs) established by European Regulation. The proposed method was applied to determine pesticide residues in commercial leafy vegetables (lettuce, Swiss chard and spinach) purchased from markets in Orense (NW Spain). Pesticide residues were detected in 84% of the total samples (63 from 75 samples) and pesticide concentrations were higher than MRL in 18 samples. PMID:18343389

  3. Analysis of organochlorine pesticides in coral (Porites evermanni) samples using accelerated solvent extraction and gas chromatography/ion trap mass spectrometry.

    PubMed

    Wang, Dongli; Miao, Xiusheng; Li, Qing X

    2008-02-01

    A gas chromatography/ion trap mass spectrometry method was developed for analysis of organochlorine pesticides (OCPs) in coral samples, which were extracted with accelerated solvent extraction (ASE) and cleaned up on a sulfuric acid-modified silica gel column. The optimal ASE conditions were found to be 100 degrees C and 2000 psi, with a mixture of acetone and methylene chloride (1:1, v/v). The target analytes include hexachlorocyclohexanes (HCHs, specifically, alpha-, beta-, gamma-, and delta-HCH isomers), heptachlor, and hexachlorobenzene (HCB), o,p'-, p,p'-dichlorodiphenyltrichloroethane (o,p'-, p,p'-DDT), o,p'-, p,p'-dichlorodiphenyl-dichloroethylene (o,p'-, p,p'-DDE), and o,p'-, p,p'-dichlorodiphenyldichloroethane (o,p'-, p,p'-DDD). Standard sand samples were used as an alternative matrix spiked with OCP standards to determine the method precision and accuracy. Average recoveries of OCPs ranged from 82% to 102%, with relative standard deviations (RSDs) of 3%-6%, at a level of 10 ng/g and from 50% to 68%, with RSDs of 13%-19% at a level of 2 ng/g. The developed method was applied for analysis of OCPs in coral samples collected from Tern Island and Bikini Atoll in the Pacific Ocean. The concentrations of HCB were 7-26 pg/g dry weight in the samples from Bikini Atoll and 3-45 pg/g in those from Tern Island, and heptachlor concentrations were 208-2200 and 44-104 pg/g in the coral samples from Bikini Atoll and Tern Island, respectively. (summation operator)HCH (sum of alpha-, beta-, gamma-, and delta-HCH) were 8-82 pg/g in Bikini Atoll coral and 86-629 pg/g in Tern island coral, and (summation operator)DDT (sum of o,p'-, p,p'-DDD, o,p'-, p,p'-DDE, and o,p'- p,p'-DDT) were 80-212 pg/g in Bikini Atoll coral and 593-3165 pg/g in Tern Island coral. The results suggest that coral is a viable indicator species for pollution monitoring, which pollutants and their concentrations may be related to dated carbonate layers. PMID:17721673

  4. Comparative study of comprehensive gas chromatography-nitrogen chemiluminescence detection and gas chromatography-ion trap-tandem mass spectrometry for determining nicotine and carcinogen organic nitrogen compounds in thirdhand tobacco smoke.

    PubMed

    Ramírez, Noelia; Vallecillos, Laura; Lewis, Alastair C; Borrull, Francesc; Marcé, Rosa M; Hamilton, Jacqueline F

    2015-12-24

    Thirdhand tobacco smoke (THS) constitutes a poorly understood pathway of exposure of non-smokers, especially toddlers, to tobacco-related carcinogens. However, to date most of the carcinogens present in tobacco smoke have not been detected in THS and, therefore, the significance of THS health risk is still unknown. In this study, we have compared the performance of two analytical methods - one based on gas chromatography coupled to ion trap mass spectrometry detection (GC-IT-MS) and the other on comprehensive two-dimensional gas chromatography coupled to a nitrogen chemiluminescence detector (GC×GC-NCD) - for simultaneously determining, in settled house dust, the presence of 16 organic nitrogen carcinogens already detected in tobacco smoke. The target compounds included four aromatic amines, two nitrocompounds, eight N-nitrosamines and two tobacco-specific nitrosamines, as well as nicotine as a tobacco marker. Dust samples were extracted using in-cell clean up pressurized liquid extraction with silica as clean up sorbent and ethyl acetate as the organic solvent, with average recovery of 89%. Although GC-IT-MS, using chemical ionization with methanol and tandem MS, performed well, the optimized GC×GC-NCD gave lower limits of detection (from 4 to 22ngg(-1)) and better repeatability and reproducibility a low concentration levels (%RSD<8%) and, therefore, was applicable for determining these different groups of carcinogens without the need for derivatization prior to the GC analysis. The performance of the optimized PLE/GC×GC-NCD method was tested by quantifying the target compounds in house dust samples from smokers' and non-smokers' homes. The median carcinogen compounds detected was 3.8μgg(-1) and 1.1μgg(-1) in smokers' and non-smokers' house dust, respectively. In this study, we have detected highly carcinogenic aromatic amines and nitro compounds for the first time in settled house dust complementing the state of knowledge of THS composition and providing

  5. Multiwalled carbon nanotubes as a solid-phase extraction adsorbent for the determination of three barbiturates in pork by ion trap gas chromatography-tandem mass spectrometry (GC/MS/MS) following microwave assisted derivatization.

    PubMed

    Zhao, Haixiang; Wang, Liping; Qiu, Yueming; Zhou, Zhiqiang; Zhong, Weike; Li, Xiang

    2007-03-14

    A new method was developed for the rapid screening and confirmation analysis of barbital, amobarbital and phenobarbital residues in pork by gas chromatography-tandem mass spectrometry (GC/MS/MS) with ion trap MSD. The residual barbiturates in pork were extracted by ultrasonic extraction, cleaned up on a multiwalled carbon nanotubes (MWCNTs) packed solid phase extraction (SPE) cartridge and applied acetone-ethyl acetate (3:7, v/v) mixture as eluting solvent and derivatized with CH3I under microwave irradiation. The methylated barbiturates were separated on a TR-5MS capillary column and detected with an ion trap mass detector. Electron impact ion source (EI) operating MS/MS mode was adopted for identification and external standard method was employed for quantification. One precursor ion m/z 169 was selected for analysis of barbital and amobarbital and m/z 232 was selected for phenobarbital. The product ions were obtained under 1.0 V excitation voltage. Good linearities (linear coefficient R > 0.99) were obtained at the range of 0.5-50 microg kg(-1). Limit of detection (LOD) of barbital was 0.2 microg kg(-1) and that of amobarbital and phenobarbital were both 0.1 microg kg(-1) (S/N > or = 3). Limit of quantification (LOQ) was 0.5 microg kg(-1) for three barbiturates (S/N > or = 10). Satisfying recoveries ranging from 75% to 96% of the three barbiturates spiked in pork were obtained, with relative standard deviations (R.S.D.) in the range of 2.1-7.8%. PMID:17386740

  6. Determination of microbial volatile organic compounds from Staphylococcus pasteuri against Tuber borchii using solid-phase microextraction and gas chromatography/ion trap mass spectrometry.

    PubMed

    Barbieri, E; Gioacchini, A M; Zambonelli, A; Bertini, L; Stocchi, V

    2005-01-01

    The mycelium of Tuber borchii Vittad., a commercial truffle species, is used as a model system for in vitro ectomycorrhizal synthesis, infected seedling production and biotechnological applications. Our fungal cultures were accidentally contaminated with a Staphylococcus pasteuri strain, showing a strong antifungal activity against T. borchii mycelium. In order to identify the antifungal volatile agents produced by S. pasteuri, solid-phase microextraction (SPME) with gas chromatography and mass spectrometry (GC/MS) was used. Using this method 65 microbial volatile organic compounds (MVOCs), synthesized by this bacterium in either single or in fungal-bacterial dual culture, were identified. SPME combined with GC/MS may be a useful method for the determination of MVOCs involved in the antifungal activity. These results showed that bacteria with unusual biological activities could be a major problem during large-scale production of inoculum for truffle-infected seedling. PMID:16259047

  7. Suitability of magnetic particle immunoassay for the analysis of PBDEs in Hawaiian freshwater fish and crabs in comparison with gas chromatography/electron capture detection-ion trap mass spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A gas chromatograph/electron capture detector-ion trap mass spectrometer (GC/ECD-ITMS) was used for the determination of polybrominated diphenyl ethers (PBDEs) in freshwater fish and crabs. The samples were also analyzed with an enzyme-linked immunosorbent assay (ELISA). GC/ECD-ITMS results showed...

  8. Validation of an analytical method for analysis of cannabinoids in hair by headspace solid-phase microextraction and gas chromatography-ion trap tandem mass spectrometry.

    PubMed

    Emídio, Elissandro Soares; Prata, Vanessa de Menezes; Dórea, Haroldo Silveira

    2010-06-18

    The development of an analytical method for the determination of Delta(9)-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in samples of human hair is described. Samples were subjected to a procedure based on the combination of headspace solid-phase microextraction (HS-SPME) with gas chromatography linked with mass spectrometry operating in tandem mode (GC-MS/MS). A 10 mg aliquot of sample was firstly decontaminated using petroleum ether, deionized water and dichloromethane (2 mL of each solvent), for 10 min under sonication, and then digested in alkaline solution (1 mol L(-1) NaOH). The method variables evaluated were pH, mass of hair, fiber type, extraction temperature, desorption time, ionic strength, pre-equilibrium time and extraction time. Parameters concerning operation of the tandem mode MS/MS were also assessed and optimized. Validation of the method demonstrated excellent linearity in the range 0.1-8.0 ng mg(-1), with regression coefficients better than 0.994. Precision was determined using two different concentrations (upper and lower limits of the linear range), and RSD values were between 6.6 and 16.4%. Absolute recoveries (measured in triplicate) were in the range 1.1-8.7%, and limits of detection and quantification were 0.007-0.031 ng mg(-1) and 0.012-0.062 ng mg(-1), respectively. The LOQ for THC (0.062 ng mg(-1)) was below the cut-off value (LOQ < or = 0.1 ng mg(-1)) established by the Society of Hair Testing (SOHT), the Society of Toxicological and Forensic Chemistry (STFCh) and the Société Française de Toxicologie Analytique (SFTA). The optimized SPME method was applied in analysis of hair samples from Cannabis drug users, showing that CBN and CBD were present in all samples analyzed. PMID:20685418

  9. Rapid and simple determination of acrylamide in conventional cereal-based foods and potato chips through conversion to 3-[bis(trifluoroethanoyl)amino]-3-oxopropyl trifluoroacetate by gas chromatography coupled with electron capture and ion trap mass spectrometry detectors.

    PubMed

    Russo, Mario Vincenzo; Avino, Pasquale; Centola, Angela; Notardonato, Ivan; Cinelli, Giuseppe

    2014-03-01

    A new, simple, rapid and fully validated method based on gas chromatography coupled with Electron capture and ion trap mass spectrometry detectors (GC-ECD and GC-IT/MS) is presented for quantitative analysis of acrylamide contaminant in conventional cereal-based foods and potato chips. Before analysis acrylamide was efficiently derivatized with trifluoroacetic anhydride, the effects of temperature, reaction time and catalyst on the acylation reaction were evaluated. Chromatographic analysis was performed on SE-54 capillary column; good retention and peak response of the acrylamide derivative achieved under the optimal conditions. The analytical method has been fully validated by assessment of the following parameters: LODs and LOQs (1 and 25ngg(-1) by GC-ECD and 2 and 36ngg(-1) by GC-IT/MS, with a Relative Standard Deviations <4 and <6, respectively), linearity (R(2) above 0.981 in the range 0.005-50μgg(-1)) and extraction recovery (ranging between 91% and 99%, RSD below 4.0, for acrylamide spiked at levels of 1, 20, 50 and 100ngg(-1)). Furthermore, the method proposed requires no clean-up step of the acrylamide derivative to be performed prior to injection. The developed method has been successfully applied to determine acrylamide in different commercial cereal-based foods (including French fries and potato chips). PMID:24176333

  10. Quantitative determination of sotolon, maltol and free furaneol in wine by solid-phase extraction and gas chromatography-ion-trap mass spectrometry.

    PubMed

    Ferreira, Vicente; Jarauta, Idoia; López, Ricardo; Cacho, Juan

    2003-08-22

    A method for the analytical determination of sotolon [4,5-dimethyl-3-hydroxy-2(5H)-furanone], maltol [3-hydroxy-2-methyl-4H-pyran-4-one] and free furaneol [2,5-dimethyl-4-hydroxy-3(2H)-furanone] in wine has been developed. The analytes are extracted from 50 ml of wine in a solid-phase extraction cartridge filled with 800 mg of LiChrolut EN resins. Interferences are removed with 15 ml of a pentane-dichloromethane (20:1) solution, and analytes are recovered with 6 ml of dichloromethane. The extract is concentrated up to 0.1 ml and analyzed by GC-ion trap MS. Maltol and sotolon were determined by selected ion storage of ions in the m/z ranges 120-153 and 79-95, using the ions m/z 126 and 83 for quantitation, respectively. Furaneol was determined by non-resonant fragmentation of the m/z 128 mother ion and subsequent analysis of the m/z 81 ion. The detection limits of the method are in all cases between 0.5 and 1 microg l(-1), well below the olfactory thresholds of the compounds. The precision of the method is in the 4-5% range for levels in wine around 20 microg l(-1). Linearity holds at least up to 400 microg l(-1), and is satisfactory in all cases. The recoveries of maltol and sotolon are constant (70 and 64%, respectively) and do not depend on the type of wine. On the contrary, in the case of furaneol, red wines show constant and high recoveries (97%), while the recoveries on white wines range between 30 and 80%. Different experiments showed that this behavior is probably due to the existence of complexes formed between furaneol and sulphur dioxide or catechols. Sensory experiments confirmed that the complexed forms found in white wines are not perceived by orthonasal olfaction, and that the furaneol determined by the method can be considered as the free and odor-active fraction. PMID:14503819

  11. Simultaneous use of gas chromatography/ion trap mass spectrometry - electron capture detector to improve the analysis of bromodiphenyl ethers in biological and environmental samples

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The mass range limit of some gas chromatograph/mass spectrometers (GC/MS) prohibits the sensitive analysis of higher brominated diphenyl ethers (BDEs). A gas chromatograph/electron capture detector (GC/ECD) can sensitively determine higher BDEs. In this study, a method that GC eluents were split wit...

  12. Miniaturized gas chromatograph-Paul ion trap system: applications to environmental monitoring

    NASA Technical Reports Server (NTRS)

    Shortt, B. J.; Darrach, M. R.; Holland, Paul M.; Chutjian, A.

    2004-01-01

    A miniature gas chromatograph (GC) and miniature Paul ion trap (PT) mass spectrometer system has been developed for identifying and quantifying chemical species present in closed environments having a complex mixture of gases.

  13. Multiresidue determination of 11 new fungicides in grapes and wines by liquid-liquid extraction/clean-up and programmable temperature vaporization injection with analyte protectants/gas chromatography/ion trap mass spectrometry.

    PubMed

    González-Rodríguez, Rosa M; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2009-08-01

    A gas chromatographic ion trap mass spectrometry (GC-ITMS) method was developed for the determination of 11 new generation fungicides (benalaxyl, benalaxyl-M, boscalid, cyazofamid, famoxadone, fenamidone, fluquinconazole, iprovalicarb, pyraclostrobin, trifloxystrobin and zoxamide) in grapes and wines. Samples were extracted with ethyl acetate:hexane (1:1, v/v) and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The addition of analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid gamma-lactone) in the final extracts allowed to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 16% for all fungicides. Limits of detection and quantitation were lower than 0.01 mg/kg or mg/L, except for cyazofamid, much smaller in all cases than maximum residue levels (MRLs) established by European Union for grapes and by Switzerland and Italy for wines. The proposed method was applied to determine fungicide residues in three different white grapes for vinification produced in Ribeiro area in Galicia (NW Spain), as well as in their corresponding final wines. PMID:19576591

  14. Quantitative determination of medroxyprogesterone acetate in plasma by liquid chromatography/electrospray ion trap mass spectrometry.

    PubMed

    Kim, S M; Kim, D H

    2001-01-01

    A sensitive and rapid liquid chromatography/electrospray ion trap mass spectrometry (LC/MS/MS) method has been developed for the quantitative determination of medroxyprogesterone acetate (MPA) in human plasma. Plasma samples (1.0 mL) were simply extracted with pentane and the extracts were analyzed by HPLC with the detection of the analyte in the selective reaction monitoring (SRM) mode. The determination of MPA was accurate and reproducible, with a limit of quantitation of 0.05 ng/mL in plasma. The standard calibration curve for MPA was linear (r = 0.998) over the concentration range 0.05-6.0 ng/mL in human plasma. Analysis precision over the concentration range of MPA was lower than 18.8% (relative standard deviation, RSD) and accuracy was between 96.2 and 108.7%. PMID:11675672

  15. Miniaturized system of a gas chromatograph coupled with a Paul ion trap mass spectrometer

    NASA Technical Reports Server (NTRS)

    Shortt, B. J.; Darrach, M. R.; Holland, Paul M.; Chutjian, A.

    2005-01-01

    Miniature gas chromatography (GC) and miniature mass spectrometry (MS) instrumentation has been developed to identify and quantify the chemical compounds present in complex mixtures of gases. The design approach utilizes micro-GC components coupled with a Paul quadrupole ion trap (QIT) mass spectrometer. Inherent to the system are high sensitivity, good dynamic range, good QIT resolution, low GC flow-rates to minimize vacuum requirements and the need for consumables; and the use of a modular approach to adapt to volatile organic compounds dissolved in water or present in sediment. Measurements are reported on system response to gaseous species at concentrations varying over four orders of magnitude. The ability of the system to deal with complicated mixtures is demonstrated, and future improvements are discussed. The GC/QIT system described herein has a mass, volume and power that are, conservatively, one-twentieth of those of commercial off-the-shelf systems. Potential applications are to spacecraft cabin-air monitoring, robotic planetary exploration and trace-species detection for residual gas analysis and environmental monitoring.

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

    PubMed

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

    2013-12-15

    Enniatins A, A1, B and B1 (ENs) are mycotoxins produced by Fusarium spp. and are normal contaminants of cereals and derivate products. In this study, the stability of ENs was evaluated during food processing by simulation of pasta cooking. Thermal treatments at different incubation times (5, 10 and 15 min) and different pH (4, 7 and 10) were applied in an aqueous system and pasta resembling system (PRS). The concentrations of the targeted mycotoxins were determined using liquid chromatography coupled to tandem mass spectrometry. High percentages of ENs reduction (81-100%) were evidenced in the PRS after the treatments at 5, 10 and 15 min of incubation. In contrast to the PRS, an important reduction of the ENs was obtained in the aqueous system after 15 min of incubation (82-100%). In general, no significant differences were observed between acid, neutral and basic solutions. Finally, several ENs degradation products were identified using the technique of liquid chromatography-triple quadrupole linear ion trap mass spectrometry. PMID:23993608

  17. Tailored Noise Waveform/ Collision-Induced Dissociation of Ions Stored in a Linear Ion Trap Combined with Liquid Chromatography/Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    SciTech Connect

    Vilkov, Andrey N.; Bogdanov, Bogdan; Pasa-Tolic, Liljiana; Prior, David C.; Anderson, Gordon A.; Masselon, Christophe D.; Moore, Ronald J.; Smith, Richard D.

    2004-11-01

    A new collision-induced dissociation (CID) technique based on broadband tailored noise waveform (TNW) excitation of ions stored in a linear ion trap has been developed. In comparison with the conventional sustained off-resonance irradiation (SORI) CID method commonly used in Fourier transform ion cyclotron resonance mass spectrometry, this MS/MS technique increases throughput by eliminating the long pump-down delay associated with gas introduction into the high vacuum ICR cell region. In addition, the TNW-CID method speeds spectrum acquisition since it does not require Fourier transformation, calculation of resonant frequencies and generation of the excitation waveforms. We demonstrate TNW-CID coupled with on-line capillary reverse phase liquid chromatography separations for identification of peptides. The experimental results are compared with data obtained using conventional quadrupole ion trap MS/MS and SORI-CID MS/MS in an ICR cell.

  18. Characterization of impurities in tylosin using dual liquid chromatography combined with ion trap mass spectrometry.

    PubMed

    Chopra, Shruti; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

    2013-03-15

    Investigation of unknown impurities in a tylosin sample was performed using liquid chromatography coupled to mass spectrometry (LC/MS). Separation was performed according to the recently described LC-UV method of Ashenafi et al. (2011) [14]. This method was reported to have a good selectivity as it was able to separate the four main components of tylosin from the already known and 23 unknown impurities. However, as this method uses a mobile phase with non-volatile constituents, direct characterization of these impurities using LC/MS was not possible. The impurity fractions were therefore first collected and then desalted before sending them to the MS. Identification of the impurities in the tylosin sample was performed with a quadruple ion trap (IT) MS, with an electrospray ionization (ESI) source in the positive ion mode. The structure of the impurities was deduced by comparing their fragmentation pattern with those of the main components of tylosin. As several peaks in the LC-UV method contained multiple compounds, using this method in total 41 new impurities were (partly) characterized. PMID:23598092

  19. A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extraction and gas chromatography-ion trap mass spectrometry

    USGS Publications Warehouse

    Hladik, M.L.; Smalling, K.L.; Kuivila, K.M.

    2008-01-01

    A method was developed for the analysis of over 60 pesticides and degradates in water by HLB solid-phase extraction and gas-chromatography/mass spectrometry. Method recoveries and detection limits were determined using two surface waters with different dissolved organic carbon (DOC) concentrations. In the lower DOC water, recoveries and detection limits were 80%-108% and 1-12 ng/L, respectively. In the higher DOC water, the detection limits were slightly higher (1-15 ng/L). Additionally, surface water samples from four sites were analyzed and 14 pesticides were detected with concentrations ranging from 4 to 1,200 ng/L. ?? 2008 Springer Science+Business Media, LLC.

  20. ANALYSIS FOR B-LACTAM ANTIBIOTICS IN KIDNEY TISSUE BY LIQUID CHROMATOGRAPHY WITH ELECTROSPRAY IONIZATION AND SELECTIVE REACTION MONITORING/TANDEM ION TRAP MASS SPECTROMETRY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Eleven B-lactams antibiotics were analyzed in fortified and incurred beef kidney tissue using high-performance liquid chromatography/selective reaction monitoring/tandem ion trap mass spectrometry. The analytes included: deacetylcephapirin, amoxicillin, cephapirin, desfuroylceftiofur cysteine disul...

  1. Electrospray liquid chromatography quadrupole ion trap mass spectrometry determination of phenyl urea herbicides in water.

    PubMed

    Draper, W M

    2001-06-01

    Phenyl urea herbicides were determined in water by electrospray quadrupole ion trap liquid chromatography-mass spectrometry (ES-QIT-LC-MS). Over a wide concentration range [M - H](-) and MH(+) ions were prominent in ES spectra. At high concentrations dimer and trimer ions appeared, and sodium, potassium, and ammonium adducts also were observed. In the case of isopturon, source collision-induced dissociation (CID) fragmentation with low offset voltages increased the ion current associated with MH(+) and diminished dimer and trimer ion abundance. In the mass analyzer CID involved common pathways, for example, daughter ions of [M - H](-) resulted from loss of R(2)NH in N',N'-dialkyl ureas or loss of C(3)H(5)NO(2) (87 amu) in N'-methoxy ureas. A 2 mm (i.d.) x 15 cm C(18) reversed phase column was used for LC-MS with a linear methanol/water gradient and 0.5 mL/min flow rate. Between 1 and 100 pg/microg/L the response was highly linear with instrument detection limits ranging from <10 to 50 pg injected. Whereas the positive ES signal intensity was greater for each of the compounds except fluometuron, negative ion monitoring gave the highest signal-to-noise ratio. Analysis of spiked Colorado River water, a source high in total dissolved solids and total organic carbon, demonstrated that ES-QIT-LC-MS was routinely capable of quantitative analysis at low nanogram per liter concentrations in conjunction with a published C(18) SPE method. Under these conditions experimental method detection limits were between 8.0 and 36 ng/L, and accuracy for measurements in the 20-50 parts per trillion range was from 77 to 96%. Recoveries were slightly lower in surface water (e.g., 39-76%), possibly due to suppression of ionization. PMID:11409961

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

    PubMed

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

    2014-02-01

    A simple, precise, accurate, and validated liquid chromatography-quadrupole linear ion trap mass spectrometry method was developed for the determination of vanillin, ethyl vanillin, and coumarin in infant formula samples. Following ultrasonic extraction with methanol/water (1:1, vol/vol), and clean-up on an HLB solid-phase extraction cartridge (Waters Corp., Milford, MA), samples were separated on a Waters XSelect HSS T3 column (150 × 2.1-mm i.d., 5-μm film thickness; Waters Corp.), with 0.1% formic acid solution-acetonitrile as mobile phase at a flow rate of 0.25 mL/min. Quantification of the target was performed by the internal standard approach, using isotopically labeled compounds for each chemical group, to correct matrix effects. Data acquisition was carried out in multiple reaction monitoring transitions mode, monitoring 2 multiple reaction monitoring transitions to ensure an accurate identification of target compounds in the samples. Additional identification and confirmation of target compounds were performed using the enhanced product ion modus of the linear ion trap. The novel liquid chromatography-quadrupole linear ion trap mass spectrometry platform offers the best sensitivity and specificity for characterization and quantitative determination of vanillin, ethyl vanillin, and coumarin in infant formula and fulfills the quality criteria for routine laboratory application. PMID:24359823

  3. Broad spectrum drug screening using liquid chromatography-hybrid triple quadrupole linear ion trap mass spectrometry.

    PubMed

    Stone, Judy

    2010-01-01

    Centrifuged urine, internal standard (promazine), and ammonium formate buffer are mixed in an autosampler vial to achieve a 10-fold dilution of the specimen. Without additional pretreatment, 10 microL of the sample is injected onto a C18 reverse phase column for gradient analysis with ammonium formate/acetonitrile mobile phases. Drugs in the column eluent become charged in the ion source using positive electrospray atmospheric pressure ionization. Pseudomolecular drug ions are analyzed by a hybrid triple quadrupole linear ion trap mass spectrometer operated with a 264-drug selected ion monitoring (SRM) acquisition method that includes an information-dependant acquisition (IDA) algorithm. PMID:20077072

  4. Universal collisional activation ion trap mass spectrometry

    DOEpatents

    McLuckey, S.A.; Goeringer, D.E.; Glish, G.L.

    1993-04-27

    A universal collisional activation ion trap comprises an ion trapping means containing a bath gas and having connected thereto a noise signal generator. A method of operating a universal collisional activation ion trap comprises the steps of: providing an ion trapping means; introducing into the ion trapping means a bath gas; and, generating a noise signal within the ion trapping means; introducing into the ion trapping means a substance that, when acted upon by the noise signal, undergoes collisional activation to form product ions.

  5. Universal collisional activation ion trap mass spectrometry

    DOEpatents

    McLuckey, Scott A.; Goeringer, Douglas E.; Glish, Gary L.

    1993-01-01

    A universal collisional activation ion trap comprises an ion trapping means containing a bath gas and having connected thereto a noise signal generator. A method of operating a universal collisional activation ion trap comprises the steps of: providing an ion trapping means; introducing into the ion trapping means a bath gas; and, generating a noise signal within the ion trapping means; introducing into the ion trapping means a substance that, when acted upon by the noise signal, undergoes collisional activation to form product ions.

  6. Analysis of pesticides residues in fresh produce using buffered acetonitrile extraction and aminopropyl cleanup with gas chromatography/triple quadrupole mass spectrometry, liquid chromatography/triple quadrupole mass spectrometry, gas chromatography/ion trap detector mass spectrometry, and GC with a halogen-specific detector.

    PubMed

    Brown, Amy N; Cook, Jo Marie; Hammack, Walter T; Stepp, Jason S; Pelt, Jonathan V; Gerard, Ghislain

    2011-01-01

    A rapid and inexpensive multiresidue method for determining pesticides in fruits and vegetables is presented. Extraction of a 15 g sample with 15 mL acetonitrile was followed by buffering with magnesium sulfate, sodium chloride, sodium citrate dihydrate, and disodium citrate. Acidification with formic acid prior to dispersive cleanup with aminopropyl sorbent and magnesium sulfate was used to stabilize base-sensitive pesticides such as chlorothalonil. Extracts were concentrated to 2 g/mL. Analyses were conducted by GC/ion trap detector MS, GC-halogen-specific detector, and LC/triple quadrupole MS. Accuracy and repeatability for 166 compounds in tomato, potato, and cabbage were 70-120% and <20% CV in 85% of the compounds, respectively. Reproducibility over a 4 month period in multiple commodities and analytical conditions was 62-124%, with CVs better than 30% for 91% of the compounds. Supply cost/sample was reduced 66%, and time to extract a batch of 24 samples was reduced by half compared to the prior method that used a 50 g sample, 100 mL acetonitrile, multiple SPE columns, and additional instrumentation. Additional extraction studies were conducted in tomatoes, oranges, and green beans at 4 g/mL using a GC/MS triple quadrupole system with a programmable temperature vaporization inlet. Recoveries of 70-120% were achieved in 93% of all compounds in green beans, 95% in tomatoes, and 97% in oranges. PMID:21797022

  7. An improved thin-layer chromatography/mass spectrometry coupling using a surface sampling probe electrospray ion trap system

    SciTech Connect

    Ford, Michael J; Van Berkel, Gary J

    2004-01-01

    A combined surface sampling probe/electrospray emitter coupled with an ion trap mass spectrometer was used for the direct read out of unmodified reversed-phase C18 thin-layer chromatography (TLC) plates. The operation of the surface sampling electrospray ionization interface in positive and negative ionization modes was demonstrated through the direct analysis of TLC plates on which a commercial test mix comprised of four dye compounds viz., rhodamine B, fluorescein, naphthol blue black, and fast green FCF, and an extract of the caffeine-containing plant Ilex vomitoria, were spotted and developed. Acquisition of full-scan mass spectra and automated collection of MS/MS product ion spectra while scanning a development lane along the surface of a TLC plate demonstrated the advantages of using an ion trap in this combination. Details of the sampling system, benefits of analyzing a developed lane in both positive ion and negative ion modes, levels of detection while surface scanning, surface scan speed effects, and the utility of three-dimensional data display, are also discussed.

  8. Gas Chromatography.

    ERIC Educational Resources Information Center

    Karasek, Francis W.; And Others

    1984-01-01

    This review covers fundamental developments in gas chromatography during 1982 and 1983. Literature is considered under these headings: columns; liguid phases; solid supports; sorption processes and solvents; open tubular column gas chromatography; instrumentation; high-resolution columns and applications; other techniques; qualitative and…

  9. Comparison of liquid chromatography using triple quadrupole and quadrupole ion trap mass analyzers to determine pesticide residues in oranges.

    PubMed

    Soler, Carla; Mañes, Jordi; Picó, Yolanda

    2005-03-01

    Liquid chromatography-triple quadrupole/mass spectrometry (LC-TQ/MS) and liquid chromatography-quadrupole ion trap/mass spectrometry (LC-QIT/MS) for determining bupirimate, hexaflumuron, tebufenpyrad, buprofezin, pyriproxyfen, and fluvalinate in fruits have been compared. The differences in the mass spectra obtained by triple and ion trap quadrupoles are discussed, showing how both of them provide interesting features. The evaluation of the two instruments was carried out by ethyl acetate extraction of oranges spiked with the studied pesticides at LOQ and 10 times the LOQ. Results obtained by LC-TQ/MS correlated well with those obtained by LC-QIT/MS. Recoveries were 70-94% by LC-TQ/MS and 72-92% by LC-QIT/MS with the R.S.D. from five replicate analysis 4-14% and 8-18%, respectively. Matrix effects were tested for both techniques by standard addition to blank extracts. Although the matrix effects are not originated in mass analyzer but in the LC/MS interface, they were, generally, more marked by LC-QIT-MS than by LC-TQ/MS. The limits of quantification (LOQs) were 0.005-0.2 mg kg(-1) by both equipments--appropriate values for determining these pesticides in orange from the regulatory point of view. The results indicate that the TQ provides higher precision, better linearity, it is more robust, and when the purpose of the analysis is quantitative determination, preferable over the QIT. However, the application of both mass spectrometers to analyze orange samples conventionally treated showed that any can be used for qualitative and quantitative purposes. PMID:15844516

  10. POLAR ORGANIC CHEMICAL INTEGRATIVE SAMPLING AND LIQUID CHROMATOGRAPHY-ELECTROSPRAY/ION-TRAP MASS SPECTROMETRY FOR ASSESSING SELECTED PRESCRIPTION AND ILLICIT DRUGS IN TREATED SEWAGE EFFLUENTS

    EPA Science Inventory

    The purpose of the research presented in this paper is two-fold: (1) to demonstrate the 4 coupling of two state-of-the-art techniques: a time-weighted polar organic integrative sampler (POCIS) and micro-liquid chromatography-electrospray/ion trap mass spectrometry (u-LC-6 ES/ITMS...

  11. Gas Chromatography.

    ERIC Educational Resources Information Center

    Cram, Stuart P.; And Others

    1980-01-01

    Selects fundamental developments in theory, methodology, and instrumentation in gas chromatography (GC). A special section reviews GC in the People's Republic of China. Over 1,000 references are cited. (CS)

  12. Appropriate choice of collision-induced dissociation energy for qualitative analysis of notoginsenosides based on liquid chromatography hybrid ion trap time-of-flight mass spectrometry.

    PubMed

    Wang, Guang-Ji; Fu, Han-Xu; Xiao, Jing-Cheng; Ye, Wei; Rao, Tai; Shao, Yu-Hao; Kang, Dian; Xie, Lin; Liang, Yan

    2016-04-01

    Liquid chromatography hybrid ion trap/time-of-flight mass spectrometry possessesd both the MS(n) ability of ion trap and the excellent resolution of a time-of-flight, and has been widely used to identify drug metabolites and determine trace multi-components for in natural products. Collision energy, one of the most important factors in acquiring MS(n) information, could be set freely in the range of 10%-400%. Herein, notoginsenosides were chosen as model compounds to build a novel methodology for the collision energy optimization. Firstly, the fragmental patterns of the representatives for the authentic standards of protopanaxadiol-type and protopanaxatriol-type notoginsenosides authentic standards were obtained based on accurate MS(2) and MS(3) measurements via liquid chromatography hybrid ion trap/time-of-flight mass spectrometry. Then the extracted ion chromatograms of characteristic product ions of notoginsenosides in Panax Notoginseng Extract, which were produced under a series of collision energies and, were compared to screen out the optimum collision energies values for MS(2) and MS(3). The results demonstrated that the qualitative capability of liquid chromatography hybrid ion trap/time-of-flight mass spectrometry was greatly influenced by collision energies, and 50% of MS(2) collision energy was found to produce the highest collision-induced dissociation efficiency for notoginsenosides. BesidesAddtionally, the highest collision-induced dissociation efficiency appeared when the collision energy was set at 75% in the MS(3) stage. PMID:27114315

  13. Characterization of column packing materials in high-performance liquid chromatography by charge-detection quadrupole ion trap mass spectrometry.

    PubMed

    Xiong, Caiqiao; Zhou, Xiaoyu; Chen, Rui; Zhang, Yiming; Peng, Wen-Ping; Nie, Zongxiu; Chang, Huan-Cheng; Liu, Huwei; Chen, Yi

    2011-07-01

    This article reports an application of charge-detection quadrupole ion trap mass spectrometry (CD-ITMS) to characterize the column packing materials in high-performance liquid chromatography (HPLC). Both the mean mass and the mass distribution of the packing materials are obtained and used to calculate the specific surface area of unbonded silica, the carbon load of the bonded silica, and their particle size distributions. The obtained specific surface areas and carbon loads are consistent with those measured independently by nitrogen sorption and elemental analysis respectively, whereas the derived size distributions show better resolution than that measured by a laser particle size analyzer. Furthermore, we evaluate the uniformity of particle size, which is the key parameter for column efficiency of the liquid chromatography by analyzing the mass distribution of the packing materials at the top and bottom of the column. A broader mass distribution, which yields decreased column efficiency, is observed for the column top because of the excessive use of the column. Our results suggest that CD-ITMS can serve as an alternative means for the characterization of the packing materials in HPLC and is potentially useful for column quality control. PMID:21612293

  14. Fast carbohydrate analysis via liquid chromatography coupled with ultra violet and electrospray ionization ion trap detection in 96-well format.

    PubMed

    Rühmann, Broder; Schmid, Jochen; Sieber, Volker

    2014-07-11

    A fast carbohydrate screening platform processible in 96-well format is described. The method is suitable for the determination of various carbohydrates out of complex mixtures as obtained by acidic hydrolysis of carbohydrates polymers. The chromatographic conditions for an efficient separation (12min) and the derivatization process with 1-phenyl-3-methyl-5-pyrazolone (PMP) were optimized for high resolution separation and simultaneous determination of deoxy-, amino-, anhydro-sugars as well as hexoses, pentoses, dimers, uronic acids and degradation products like furfural and hydroxymethylfurfural (HMF). The potential to quantify with UV- and MS-detector in the same range has been demonstrated for 20 different compounds. Finally, the matrix effects of the hydrolysis were positively evaluated. The micro scale hydrolysis and PMP-derivatization without any extraction or drying steps, both in 96-well format, result in a fast and intuitive sample preparation. In combination with a fast liquid chromatography coupled to UV and electrospray ionization ion trap detection (LC-UV-ESI-MS/MS) for the qualification and quantification of various sugars, dimers and degradation products, this method shows great performance in carbohydrate analysis. PMID:24861788

  15. Identification and quantification of active alkaloids in Catharanthus roseus by liquid chromatography-ion trap mass spectrometry.

    PubMed

    Chen, Qinhua; Zhang, Wenpeng; Zhang, Yulin; Chen, Jing; Chen, Zilin

    2013-08-15

    Catharanthus roseus is an important dicotyledonous medicinal plant that produces anticancer compounds. The active alkaloids vinblastine, vindoline, ajmalicine, catharanthine, and vinleurosine were identified by direct-injection ion trap-mass spectrometry (IT-MS) for collecting MS(1-2) spectra. The determinations of five alkaloids were accomplished by liquid chromatography (LC) with UV and MS detections. The analytes provided good signals corresponding to the protonated molecular ions [M+H](+) and product ions. The precursor ions and product ions for quantification of vinblastine, vindoline, ajmalicine, catharanthine, and vinleurosine were m/z 825→807, 457→397, 353→144, 337→144 and 809→748 by LC-IT-MS, respectively. Two methods were used to evaluate a number of validation characteristics (repeatability, LOD, calibration range, and recovery). MS provided a high selectivity and sensitivity for determination of five alkaloids in positive mode. After optimisation of the methods, separation, identification and quantification of the five components in C. roseus were comprehensively accomplished by HPLC with UV and MS detection. PMID:23561180

  16. Simultaneous screening and confirmation of multiple classes of drug residues in fish by liquid chromatography-ion trap mass spectrometry.

    PubMed

    Smith, Shani; Gieseker, Charles; Reimschuessel, Renate; Decker, Christie-Sue; Carson, Mary C

    2009-11-13

    LC-ion trap mass spectrometry was used to screen and confirm 38 compounds from a variety of drug classes in four species of fish: trout, salmon, catfish, and tilapia. Samples were extracted with acetonitrile and hexane. The acetonitrile phase was evaporated, redissolved in water and acetonitrile, and analyzed by gradient chromatography on a phenyl column. MS(2) or MS(3) spectra were monitored for each compound. Qualitative method performance was evaluated by the analysis over several days of replicate samples of control fish, fish fortified with a drug mixture at 1 ppm, 0.1 ppm and 0.01 ppm, and fish dosed with a representative from each drug class. Half of the 38 drugs were confirmed at 0.01 ppm, the lowest fortification level. This included all of the quinolones and fluoroquinolones, the macrolides, malachite green, and most of the imidazoles. Florfenicol amine, metronidazole, sulfonamides, tetracyclines, and most of the betalactams were confirmed at 0.1 ppm. Ivermectin and penicillin G were only detectable in the 1 ppm fortified samples. With the exception of amoxicillin, emamectin, metronidazole, and tylosin, residue presence was confirmed in all the dosed fish. PMID:19616215

  17. Broad-Spectrum Drug Screening Using Liquid Chromatography-Hybrid Triple-Quadrupole Linear Ion Trap Mass Spectrometry.

    PubMed

    Stone, Judy

    2016-01-01

    Urine is processed with a simple C18 solid-phase extraction (SPE) and reconstituted in mobile phase. The liquid chromatography system (LC) injects 10 μL of extracted sample onto a reverse-phase LC column for gradient analysis with ammonium formate/acetonitrile mobile phases. Drugs in the column eluent become charged in the ion source using positive electrospray ionization (ESI). Pseudomolecular ions (M + H) are analyzed by a hybrid triple-quadrupole linear ion trap (QqQ and QqLIT) mass spectrometer using an SRM-IDA-EPI acquisition. An initial 125 compound selected ion monitoring (SRM) survey scan (triple quadrupole or QqQ mode) is processed by the information-dependent acquisition (IDA) algorithm. The IDA algorithm selects SRM signals from the survey scan with a peak height above the threshold (the three most abundant SRM signals above 1000 cps) to define precursor ions for subsequent dependent scanning. In the dependent QqLIT scan(s), selected precursor ion(s) are passed through the first quadrupole (Q1), fragmented with three different collision energies in the collision cell (Q2 or q), and product ions are collected in the third quadrupole (Q3), now operating as a linear ion trap (LIT). The ions are scanned out of the LIT in a mass dependent manner to produce a full-scan product ion spectrum (m/z 50-700) defined as an Enhanced (meaning acquired in LIT mode) Product Ion (EPI) spectrum (Mueller et al., Rapid Commun Mass Spectrom 19:1332-1338, 2005). Each EPI spectrum is linked to its precursor ion and to the associated SRM peak from the survey scan. EPI spectra are automatically searched against a 125 drug library of reference EPI spectra for identification. When the duty cycle is complete (one survey scan of 125 SRMs plus 0-3 dependent IDA-EPI scans) the mass spectrometer begins another survey scan of the 125 SRMs. PMID:26660183

  18. Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Qian, Michael C.; Peterson, Devin G.; Reineccius, Gary A.

    The first publication on gas chromatography (GC) was in 1952 (1), while the first commercial instruments were manufactured in 1956. James and Martin (1) separated fatty acids by GC, collected the column effluent, and titrated the individual fatty acids for quantitation. GC has advanced greatly since that early work and is now considered to be a mature field that is approaching theoretical limitations.

  19. Liquid chromatography quadrupole linear ion trap mass spectrometry for multiclass screening and identification of lipophilic marine biotoxins in bivalve mollusks.

    PubMed

    Wu, Haiyan; Guo, Mengmeng; Tan, Zhijun; Cheng, Haiyan; Li, Zhaoxin; Zhai, Yuxiu

    2014-09-01

    A liquid chromatography quadrupole linear ion trap mass spectrometry method with fast polarity switching and a scheduled multiple reaction monitoring algorithm mode was developed for multiclass screening and identification of lipophilic marine biotoxins in bivalve molluscs. A major advantage of the method is that it can detect members of all six groups of lipophilic marine biotoxins [okadaic acid (OA), yessotoxins (YTX), azaspiracids (AZA), pectenotoxins (PTX), cyclic imines (CI), and brevetoxins (PbTx)], thereby allowing quantification and high confidence identification from a single liquid chromatography tandem mass spectrometry (LC-MS/MS) injection. An enhanced product ion (EPI) library was constructed after triggered collection of data via information-dependent acquisition (IDA) of EPI spectra from standard samples. A separation method for identifying 17 target toxins in a single analysis within 12min was developed and tested. Different solid phase extraction sorbents, the matrix effect (for oyster, scallop, and mussel samples), and stability of the standards also were evaluated. Matrix-matched calibration was used for quantification of the toxins. The limits of detection were 0.12-13.6μg/kg, and the limits of quantification were 0.39-45.4μg/kg. The method was used to analyze 120 shellfish samples collected from farming areas along the coast of China, and 7% of the samples were found to be contaminated with toxins. The library search identified PbTx-3, YTX, OA, PTX2, AZA1, AZA2, and desmethylspirolide C (SPX1). Overall, the method exhibited excellent sensitivity and reproducibility, and it will have broad applications in the monitoring of lipophilic marine biotoxins. PMID:25086754

  20. Characterization of dihydrostreptomycin-related substances by liquid chromatography coupled to ion trap mass spectrometry.

    PubMed

    Pendela, Murali; Hoogmartens, Jos; Van Schepdael, Ann; Adams, Erwin

    2009-06-01

    Dihydrostreptomycin sulphate (DHS) is a water-soluble, broad-spectrum aminoglycoside antibiotic. For quantitative analysis, the European Pharmacopoeia (Ph. Eur.) prescribes an ion-pairing liquid chromatography/ultraviolet (LC/UV) method using a C18 stationary phase. Several unknown compounds were detected in commercial samples. Hence, for characterization of these unknown peaks in a commercial DHS sample, the Ph. Eur. method was coupled to mass spectrometry (MS). However, since the Ph. Eur. method uses a non-volatile mobile phase, each peak eluted was collected and desalted before introduction into the mass spectrometer. The desalting procedure was applied to remove the non volatile salt, buffer and ion-pairing reagent in the collected fraction. In total, 20 impurities were studied and 14 of them were newly characterized. Five impurities which are already reported in the literature were also traced in this LC/UV method. PMID:19449319

  1. Generic detection of basic taxoids in wood of European Yew (Taxus baccata) by liquid chromatography-ion trap mass spectrometry.

    PubMed

    Kite, Geoffrey C; Rowe, Emily R; Veitch, Nigel C; Turner, Jill E; Dauncey, Elizabeth A

    2013-02-01

    The occurrence of the cardiotoxin taxine (comprising taxine B and several other basic taxoids) in leaves of Taxus baccata L. (European yew) is well known and has led to public concerns about the safety of eating or drinking from utensils crafted from the wood of this poisonous species. The occurrence of basic taxoids in the heartwood of T. baccata had not been examined in detail, although the bark is known to contain 2'β-deacetoxyaustrospicatine. Initial examination of heartwood extracts for 2'β-deacetoxyaustrospicatine by liquid chromatography-mass spectrometry (LC-MS) revealed the presence of this basic taxoid at about 0.0007% dry weight, using a standard isolated from bark. Analyses for taxine B, however, proved negative at the extract concentration analysed. Observing other basic taxoids within the heartwood extracts was facilitated by developing generic LC-MS methods that utilised a fragment arising from the N-containing acyl group of basic taxoids as a reporter ion. Of the various MS strategies available on a hybrid ion trap-orbitrap instrument that allowed observation of this reporter ion, combining all-ion collisions with high resolution ion filtering by the orbitrap was most effective, both in terms of the number of basic taxoids detected and sensitivity. Numerous basic taxoids, in addition to 2'β-deacetoxyaustrospicatine, were revealed by this method in heartwood extracts of T. baccata. Red wine readily extracted the basic taxoids from heartwood while coffee extracted them less efficiently. Contamination with basic taxoids could also be detected in soft cheese that had been spread onto wood. The generic LC-MS method for detecting basic taxoids complements specific methods for detecting taxine B when investigating yew poisoning cases in which the analysis of complex extracts may be required or taxine B has not been detected. PMID:23314400

  2. Ion Trap Mass Spectrometry

    SciTech Connect

    Eiden, Greg C.

    2005-09-01

    This chapter describes research conducted in a few research groups in the 1990s in which RF quadrupole ion trap mass spectrometers were coupled to a powerful atomic ion source, the inductively coupled plasma used in conventional ICP-MS instruments. Major section titles for this chapter are: RF Quadrupole Ion Traps Features of RF Quadrupole Ion Trap Mass Spectrometers Selective Ion Trapping methods Inductively Coupled Plasma Source Ion Trap Mass Spectrometers

  3. Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Qian, Michael C.

    Gas chromatography (GC) has many applications in the analysis of food products. GC has been used for the determination of fatty acids, triglycerides, cholesterol, gases, water, alcohols, pesticides, flavor compounds, and many more. While GC has been used for other food components such as sugars, oligosaccharides, amino acids, peptides, and vitamins, these substances are more suited to analysis by high performance liquid chromatography. GC is ideally suited to the analysis of volatile substances that are thermally stable. Substances such as pesticides and flavor compounds that meet these criteria can be isolated from a food and directly injected into the GC. For compounds that are thermally unstable, too low in volatility, or yield poor chromatographic separation due to polarity, a derivatization step must be done before GC analysis. The two parts of the experiment described here include the analysis of alcohols that requires no derivatization step, and the analysis of fatty acids which requires derivatization. The experiments specify the use of capillary columns, but the first experiment includes conditions for a packed column.

  4. Metabonomic Study of Biochemical Changes in Human Hair of Heroin Abusers by Liquid Chromatography Coupled with Ion Trap-Time of Flight Mass Spectrometry.

    PubMed

    Xie, Pu; Wang, Tie-jie; Yin, Guo; Yan, Yan; Xiao, Li-he; Li, Qing; Bi, Kai-shun

    2016-01-01

    Hair analysis is with the advantage of non-invasive collection and long surveillance window. The present study employed a sensitive and reliable liquid chromatography coupled with ion trap-time of flight mass spectrometry method to study the metabonomic characters in the hair of 58 heroin abusers and 72 non-heroin abusers. Results indicated that certain endogenous metabolites, such as sorbitol and cortisol, were accelerated, and the level of arachidonic acid, glutathione, linoleic acid, and myristic acid was decreased in hair of heroin abusers. The metabonomic study is helpful for further understanding of heroin addiction and clinical diagnosis. PMID:26445826

  5. Collision induced dissociation of protonated N-nitrosodimethylamine by ion trap mass spectrometry: Ultimate carcinogens in gas phase

    NASA Astrophysics Data System (ADS)

    Kulikova, Natalia; Baker, Michael; Gabryelski, Wojciech

    2009-12-01

    Collision induced dissociation of protonated N-nitrosodimethylamine (NDMA) and isotopically labeled N-nitrosodimethyl-d6-amine (NDMA-d6) was investigated by sequential ion trap mass spectrometry to establish mechanisms of gas phase reactions leading to intriguing products of this potent carcinogen. The fragmentation of (NDMA + H+) occurs via two dissociation pathways. In the alkylation pathway, homolytic cleavage of the N-O bond of N-dimethyl, N'-hydroxydiazenium ion generates N-dimethyldiazenium distonic ion which reacts further by a CH3 radical loss to form methanediazonium ion. Both methanediazonium ion and its precursor are involved in ion/molecule reactions. Methanediazonium ion showed to be capable of methylating water and methanol molecules in the gas phase of the ion trap and N-dimethyldiazenium distonic ion showed to abstract a hydrogen atom from a solvent molecule. In the denitrosation pathway, a tautomerization of N-dimethyl, N'-hydroxydiazenium ion to N-nitrosodimethylammonium intermediate ion results in radical cleavage of the N-N bond of the intermediate ion to form N-dimethylaminium radical cation which reacts further through [alpha]-cleavage to generate N-methylmethylenimmonium ion. Although the reactions of NDMA in the gas phase are different to those for enzymatic conversion of NDMA in biological systems, each activation method generates the same products. We will show that collision induced dissociation of N-nitrosodiethylamine (NDEA) and N-nitrosodipropylamine (NDPA) is also a feasible approach to gain information on formation, stability, and reactivity of alkylating agents originating from NDEA and NDPA. Investigating such biologically relevant, but highly reactive intermediates in the condensed phase is hampered by the short life-times of these transient species.

  6. [Rapid screening and confirming carcinogenic banned azo colorants in textiles by high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry].

    PubMed

    Yun, Huan; Liu, Xin; Wang, Jing; Yan, Hua; Cui, Fengyun; Zhang, Zhaohui

    2013-09-01

    A method of high performance liquid chromatography-linear ion trap/orbitrap highresolution mass spectrometry (HPLC-LTP/Orbitrap MS) was ued to screen and confirm-banned azo colorants in textiles rapidly. The analytes were reduced to carcinogenic aromatic amines with sodium dithionite in citrate buffer solution. The reduced solution was extracted bydiatomite, and loadd onto an Acquity UPLC BEH C18 column (50 mm x 2.1 MM. 1.7 microm) with a gradient elution of methanol and 0.1% (v/v) methane acid aqueous solution, and finally detected by linear ion trap/orbitrap high-resolution mass spectrometry in positive ESI mode. In mass spectrometry method, the MS spectrum of high-resolution and the collision induced dissociation (CID) spectrum of data-dependent scan mode were used for screening analysis and conformation, respectively. The calibration curves showed a good linearity in the range of 0.05 -2.00 mg/b, and the correlation coefficients (r) were higher than 0.99. By detecting spiked samples, the limits of quantification were 0.08 mg/kg for all the residues and the recoveries were in the range of 65.5% - 111.5% with the relative standard deviations (RSDs) between 0.87% and 2.49%. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analysis of carcinogenic aromatic amines in textiles. PMID:24392621

  7. Determination of non-ionic polyethoxylated surfactants in wastewater and river water by mixed hemimicelle extraction and liquid chromatography-ion trap mass spectrometry.

    PubMed

    Cantero, Manuel; Rubio, Soledad; Pérez-Bendito, Dolores

    2005-03-01

    The capability of hemimicelles-based solid phase extraction (SPE)/liquid chromatography/atmospheric pressure chemical ionisation in positive mode, ion trap mass spectrometry (LC/(APCl+-IT)-MS) for the concentration, separation and quantitation of non-ionic surfactants has been investigated. Concentration was based on the formation of mixed aggregates of analytes [alkylphenol ethoxylates (APE, octyl and nonyl) and alkyl ethoxylates (AE, C12-C16)] with the anionic surfactant sodium dodecyl sulphate (SDS) that is adsorbed on alumina. Parameters affecting SPE were investigated on the basis that hemimicelles are dynamic entities in equilibrium with the aqueous phase. The performance of ion trap mass spectrometry for MS and MS/MS quantitation of non-ionic homologues was assessed. Recoveries of analytes from wastewater influent and effluent and river water samples ranged between 91 and 98% and were found independent on the length of the alkyl chain under the optimised conditions. Anionic surfactants did not interfere to the levels found in environmental samples. The detection limits ranged between 14 and 111 ng/l for wastewater influent, 10 and 40 for wastewater effluent and 4 and 35 for river water, after concentration of 250, 500 and 750 ml of sample, respectively. The approach was applied to the determination of AE and APE in influent and effluent samples from four wastewater treatment plants and four river samples. The concentrations of individual non-ionic surfactants found ranged between 0.3 and 373 microg/l. PMID:15844521

  8. Rapid Quantification of Four Anthocyanins in Red Grape Wine by Hydrophilic Interaction Liquid Chromatography/Triple Quadrupole Linear Ion Trap Mass Spectrometry.

    PubMed

    Sun, Yongming; Xia, Biqi; Chen, Xiangzhun; Duanmu, Chuansong; Li, Denghao; Han, Chao

    2015-01-01

    The identification and quantification of four anthocyanins (cyanidin-3-O-glucoside, peonidin-3-O-glucoside, delphinidin-3-O-glucoside, and malvidin-3-O-glucoside) in red grape wine were carried out by hydrophilic interaction liquid chromatography/triple quadrupole linear ion trap MS (HILIC/QTrap-MS/MS). Samples were diluted directly and separated on a Merck ZIC HILIC column with 20 mM ammonium acetate solution-acetonitrile mobile phase. Quantitative data acquisition was carried out in the multiple reaction monitoring mode. Additional identification and confirmation of target compounds were performed using the enhanced product ion mode of the linear ion trap. The LOQs were in the range 0.05-1.0 ng/mL. The average recoveries were in the range 94.6 to 104.5%. The HILIC/QTrap-MS/MS platform offers the best sensitivity and specificity for characterization and quantitative determination of the four anthocyanins in red grape wines and fulfills the quality criteria for routine laboratory application. PMID:26651575

  9. Microfabricated ion trap array

    DOEpatents

    Blain, Matthew G.; Fleming, James G.

    2006-12-26

    A microfabricated ion trap array, comprising a plurality of ion traps having an inner radius of order one micron, can be fabricated using surface micromachining techniques and materials known to the integrated circuits manufacturing and microelectromechanical systems industries. Micromachining methods enable batch fabrication, reduced manufacturing costs, dimensional and positional precision, and monolithic integration of massive arrays of ion traps with microscale ion generation and detection devices. Massive arraying enables the microscale ion traps to retain the resolution, sensitivity, and mass range advantages necessary for high chemical selectivity. The reduced electrode voltage enables integration of the microfabricated ion trap array with on-chip circuit-based rf operation and detection electronics (i.e., cell phone electronics). Therefore, the full performance advantages of the microfabricated ion trap array can be realized in truly field portable, handheld microanalysis systems.

  10. Determination of carnitine and acylcarnitines in urine by high-performance liquid chromatography-electrospray ionization ion trap tandem mass spectrometry.

    PubMed

    Vernez, Laurence; Hopfgartner, Gérard; Wenk, Markus; Krähenbühl, Stephan

    2003-01-17

    A high-performance liquid chromatography-mass spectrometry method has been developed for the simultaneous determination of native carnitine and eight acylcarnitines in urine. The procedure uses a solid-phase extraction on a cation-exchange column and the separation is performed without derivatization within 17 min on a reversed-phase C8 column in the presence of a volatile ion-pairing reagent. The detector was an ion trap mass spectrometer and quantification was carried out in the MS-MS mode. Validation was done for aqueous standards at ranges between 0.75 and 200 micromol/l, depending on the compound. Carnitine was quantified in urine and comparison with a radioenzymatic assay gave a satisfactory correlation (R2 = 0.981). The assay could be successfully applied to the diagnostic of pathological acylcarnitines profile of metabolic disorders in urines of patients suffering from different organic acidurias. PMID:12564691

  11. Ion trap simulation tools.

    SciTech Connect

    Hamlet, Benjamin Roger

    2009-02-01

    Ion traps present a potential architecture for future quantum computers. These computers are of interest due to their increased power over classical computers stemming from the superposition of states and the resulting capability to simultaneously perform many computations. This paper describes a software application used to prepare and visualize simulations of trapping and maneuvering ions in ion traps.

  12. Investigation of the gas-phase hydrogen/deuterium exchange behavior of aromatic dicarboxylic acids in a quadrupole ion trap

    NASA Astrophysics Data System (ADS)

    Chipuk, Joseph E.; Brodbelt, Jennifer S.

    2007-11-01

    Gas-phase hydrogen/deuterium (H/D) exchange reactions of four deprotonated aromatic dicarboxylic acids (phthalic acid, isophthalic acid, terephthalic acid and 2,6-naphthalic acid) with D2O were performed in a quadrupole ion trap mass spectrometer. Experimental results showed significant differences in the rate and extent of exchange when the relative position of the carboxylic acid groups varied. Spontaneous and near complete exchange of one aromatic hydrogen atom occurred when the carboxylic acid groups were in the meta-position, whereas no additional exchange was observed for either the ortho- or para-isomers or for the structurally similar naphthalic acid. Computational investigations support the participation of several possible exchange mechanisms with the contribution of each relying heavily on the relative orientation of the acid moieties. A relay mechanism that bridges the deprotonation site and the labile hydrogen site appears to be responsible for the H/D exchange of not only the labile hydrogen atom of isophthalic acid, but also for the formation of a stable carbanion and corresponding subsequent exchange of one aromatic hydrogen atom. The impact of hydrogen bonding on the relay mechanism is demonstrated by the reaction of phthalic acid as the extent and rate of reaction are greatly retarded by the favorable interaction of the two carboxylic acid groups. Finally, a flip-flop mechanism is likely responsible for the exchange of both terephthalic acid and 2,6-naphthalic acid where the reactive sites are too remote for exchange via relay.

  13. A cylindrical quadrupole ion trap in combination with an electrospray ion source for gas-phase luminescence and absorption spectroscopy.

    PubMed

    Stockett, Mark H; Houmøller, Jørgen; Støchkel, Kristian; Svendsen, Annette; Brøndsted Nielsen, Steen

    2016-05-01

    A relatively simple setup for collection and detection of light emitted from isolated photo-excited molecular ions has been constructed. It benefits from a high collection efficiency of photons, which is accomplished by using a cylindrical ion trap where one end-cap electrode is a mesh grid combined with an aspheric condenser lens. The geometry permits nearly 10% of the emitted light to be collected and, after transmission losses, approximately 5% to be delivered to the entrance of a grating spectrometer equipped with a detector array. The high collection efficiency enables the use of pulsed tunable lasers with low repetition rates (e.g., 20 Hz) instead of continuous wave (cw) lasers or very high repetition rate (e.g., MHz) lasers that are typically used as light sources for gas-phase fluorescence experiments on molecular ions. A hole has been drilled in the cylinder electrode so that a light pulse can interact with the ion cloud in the center of the trap. Simulations indicate that these modifications to the trap do not significantly affect the storage capability and the overall shape of the ion cloud. The overlap between the ion cloud and the laser light is basically 100%, and experimentally >50% of negatively charged chromophore ions are routinely photodepleted. The performance of the setup is illustrated based on fluorescence spectra of several laser dyes, and the quality of these spectra is comparable to those reported by other groups. Finally, by replacing the optical system with a channeltron detector, we demonstrate that the setup can also be used for gas-phase action spectroscopy where either depletion or fragmentation is monitored to provide an indirect measurement on the absorption spectrum of the ion. PMID:27250388

  14. A cylindrical quadrupole ion trap in combination with an electrospray ion source for gas-phase luminescence and absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Stockett, Mark H.; Houmøller, Jørgen; Støchkel, Kristian; Svendsen, Annette; Brøndsted Nielsen, Steen

    2016-05-01

    A relatively simple setup for collection and detection of light emitted from isolated photo-excited molecular ions has been constructed. It benefits from a high collection efficiency of photons, which is accomplished by using a cylindrical ion trap where one end-cap electrode is a mesh grid combined with an aspheric condenser lens. The geometry permits nearly 10% of the emitted light to be collected and, after transmission losses, approximately 5% to be delivered to the entrance of a grating spectrometer equipped with a detector array. The high collection efficiency enables the use of pulsed tunable lasers with low repetition rates (e.g., 20 Hz) instead of continuous wave (cw) lasers or very high repetition rate (e.g., MHz) lasers that are typically used as light sources for gas-phase fluorescence experiments on molecular ions. A hole has been drilled in the cylinder electrode so that a light pulse can interact with the ion cloud in the center of the trap. Simulations indicate that these modifications to the trap do not significantly affect the storage capability and the overall shape of the ion cloud. The overlap between the ion cloud and the laser light is basically 100%, and experimentally >50% of negatively charged chromophore ions are routinely photodepleted. The performance of the setup is illustrated based on fluorescence spectra of several laser dyes, and the quality of these spectra is comparable to those reported by other groups. Finally, by replacing the optical system with a channeltron detector, we demonstrate that the setup can also be used for gas-phase action spectroscopy where either depletion or fragmentation is monitored to provide an indirect measurement on the absorption spectrum of the ion.

  15. An optimized method for the determination of perfluorooctanoic acid, perfluorooctane sulfonate and other perfluorochemicals in different matrices using liquid chromatography/ion-trap mass spectrometry.

    PubMed

    Dolman, Sebastiaan; Pelzing, Matthias

    2011-07-15

    Perfluorochemicals (PFC's) are widely spread in the environment and have been detected in blood of wildlife and humans world-wide. Recently, various toxic effects of PFC's in laboratory rats have been demonstrated, resulting in increased government concerns regarding the presence of PFC's in the environment and the implications they have on human health. In the last decade, various analytical methods have been developed for the analysis of PFC's in different matrices whereby the majority of methods have utilised liquid chromatography coupled with mass spectrometry (LC-MS). Here we describe an optimized method for the quantitation of PFC's, including perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS), in food packaging, polytetrafluoroethylene (PTFE) sealant tape and drinking water. The method involved PFC's extraction via off-line SPE followed by separation using reversed-phase liquid chromatography on a Phenyl-Hexyl column coupled with ion-trap (IT) mass spectrometric detection. The optimized approach minimized ion-suppression effects commonly seen with conventional elution buffers, improving detection limits down to 25 pg/mL and allowed effective quantitation down to 50 pg/mL for PFOA and PFOS. The optimized LC-MS method detected PFOA and other PFC's in microwave popcorn packaging and PFOA in PTFE sealant tape in the low μg/kg. In all samples, PFOS was not detected. PMID:21700512

  16. Microfabricated cylindrical ion trap

    DOEpatents

    Blain, Matthew G.

    2005-03-22

    A microscale cylindrical ion trap, having an inner radius of order one micron, can be fabricated using surface micromachining techniques and materials known to the integrated circuits manufacturing and microelectromechanical systems industries. Micromachining methods enable batch fabrication, reduced manufacturing costs, dimensional and positional precision, and monolithic integration of massive arrays of ion traps with microscale ion generation and detection devices. Massive arraying enables the microscale cylindrical ion trap to retain the resolution, sensitivity, and mass range advantages necessary for high chemical selectivity. The microscale CIT has a reduced ion mean free path, allowing operation at higher pressures with less expensive and less bulky vacuum pumping system, and with lower battery power than conventional- and miniature-sized ion traps. The reduced electrode voltage enables integration of the microscale cylindrical ion trap with on-chip integrated circuit-based rf operation and detection electronics (i.e., cell phone electronics). Therefore, the full performance advantages of microscale cylindrical ion traps can be realized in truly field portable, handheld microanalysis systems.

  17. This-layer chromatography/electrospray ionization triple-quadrupole linear ion trap mass spectrometry system: analysis of rhodamine dyes separated on reversed-phase C8 plates

    SciTech Connect

    Ford, Michael J; Kertesz, Vilmos; Van Berkel, Gary J

    2005-01-01

    The direct analysis of separated rhodamine dyes on reversed-phase C{sub 8} thin-layer chromatography plates using a surface sampling/electrospray emitter probe coupled with a triple-quadrupole linear ion trap mass spectrometer is presented. This report represents continuing work to advance the performance metrics and utility of this basic surface sampling electrospray mass spectrometry system for the analysis of thin-layer chromatography plates. Experimental results examining the role of sampling probe spray end configuration on liquid aspiration rate and gas-phase ion signal generated are discussed. The detection figures-of-merit afforded by full-scan, automated product ion and selected reaction monitoring modes of operation were examined. The effect of different eluting solvents on mass spectrum signal levels with the reversed-phase C{sub 8} plate was investigated. The combined effect of eluting solvent flow-rate and development lane surface scan rate on preservation of chromatographic resolution was also studied. Analysis of chromatographically separated red pen ink extracts from eight different pens using selected reaction monitoring demonstrated the potential of this surface sampling electrospray mass spectrometry system for targeted compound analysis with real samples.

  18. Analysis of 40 weight loss compounds adulterated in health supplements by liquid chromatography quadrupole linear ion trap mass spectrometry.

    PubMed

    Zeng, Yun; Xu, Yimin; Kee, Chee-Leong; Low, Min-Yong; Ge, Xiaowei

    2016-03-01

    In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) with scheduled multiple reaction monitoring (MRM) enhanced product ion (EPI) method was developed for simultaneous determination of 40 compounds with weight loss effect, including bisacodyl, phenolphthalein, and sibutramine and its metabolites, etc. They might be adulterated in health supplements to get prominent weight loss effect. The samples were analyzed using a Q-Trap 5500 coupled with high performance liquid chromatography (HPLC) and a CORTECS ultra performance liquid chromatography (UPLC) C18 column (100 mm x 2.1 mm x1.6 µm). Scheduled MRM was used as survey scan, MS2 spectra acquired in the EPI mode were used to perform library searching to increase the confidence of detection. Limits of detection were less than 10 ng/g for the majority of the analytes. A total of 447 weight loss products were tested in our laboratory in the past three years. Among these samples, 119 samples were found to be adulterated with one or more weight loss compounds, including sibutramine, its metabolites benzyl sibutramine and desmethyl sibutramine; phenolphthalein; bisacodyl; furosemide; liothyronine (T3); and thyroxine (T4). Copyright © 2015 John Wiley & Sons, Ltd. PMID:26305055

  19. Ion Sponge: A 3-Dimentional Array of Quadrupole Ion Traps for Trapping and Mass-Selectively Processing Ions in Gas Phase

    PubMed Central

    2015-01-01

    In this study, the concept of ion sponge has been explored for developing 3D arrays of large numbers of ion traps but with simple configurations. An ion sponge device with 484 trapping units in a volume of 10 × 10 × 3.2 cm has been constructed by simply stacking 9 meshes together. A single rf was used for trapping ions and mass-selective ion processing. The ion sponge provides a large trapping capacity and is highly transparent for transfer of ions, neutrals, and photons for gas phase ion processing. Multiple layers of quadrupole ion traps, with 121 trapping units in each layer, can operate as a single device for MS or MS/MS analysis, or as a series of mass-selective trapping devices with interlayer ion transfers facilitated by AC and DC voltages. Automatic sorting of ions to different trapping layers based on their mass-to-charge (m/z) ratios was achieved with traps of different sizes. Tandem-in-space MS/MS has also been demonstrated with precursor ions and fragment ions trapped in separate locations. PMID:24758328

  20. An integrated approach for profiling oxidative metabolites and glutathione adducts using liquid chromatography coupled with ultraviolet detection and triple quadrupole-linear ion trap mass spectrometry.

    PubMed

    Chen, Guiying; Cheng, Zhongzhe; Zhang, Kerong; Jiang, Hongliang; Zhu, Mingshe

    2016-09-10

    The use of liquid chromatography (LC) coupled with triple quadrupole linear ion trap (Qtrap) mass spectrometry (MS) for both quantitative and qualitative analysis in drug metabolism and pharmacokinetic studies is of great interest. Here, a new Qtrap-based analytical methodology for simultaneous detection, structural characterization and semi-quantitation of in vitro oxidative metabolites and glutathione trapped reactive metabolites was reported. In the current study, combined multiple ion monitoring and multiple reaction monitoring were served as surveying scans to trigger product ion spectral acquisition of oxidative metabolites and glutathione adduct, respectively. Then, detection of metabolites and recovery of their MS/MS spectra were accomplished using multiple data mining approaches. Additionally, on-line ultraviolet (UV) detection was employed to determine relative concentrations of major metabolites. Analyses of metabolites of clozapine and nomifensine in rat liver microsomes not only revealed multiple oxidative metabolites and glutathione adducts, but also identified their major oxidative metabolism and bioactivation pathways. The results demonstrated that the LC/UV/MS method enabled Qtrap to perform the comprehensive profiling of oxidative metabolites and glutathione adducts in vitro. PMID:27497649

  1. Ultra-high-performance liquid chromatography-ion trap mass spectrometry characterisation of milk polar lipids from dairy cows fed different diets.

    PubMed

    Craige Trenerry, V; Akbaridoust, Ghazal; Plozza, Tim; Rochfort, Simone; Wales, William J; Auldist, Martin; Ajlouni, Said

    2013-11-15

    Milk polar lipids are an important class of biologically active species for human health and for improving the physical functionality of food ingredients. Milk polar lipids from 144 multiparous Holstein-Friesian dairy cows fed different diets were analysed using ultra-high-performance liquid chromatography-ion trap mass spectrometry (UHPLC-MS(n)). A complex profile of polar lipids, consisting of 7 species of phosphatidylinositol (PI), 12 species of phosphatidylethanolamine (PE), 18 species of phosphatidylcholine (PC) and 13 species of sphingomyelin (SM) were identified from the molecular ions and sequential MS(n) fragmentation. Qualitative assessment of the data suggested that different cow diets influenced the relative amounts of a small number of species in the milk samples, e.g. PE 14:0/18:1, PE 18:0/18:1, PC 15:0/18:1, PC 18:0/18:1, SM d18:1/14:0, SM d18:1/15:0, SM d18:1/22:0 and SM d18:1/23:0. PMID:23790938

  2. Analysis of veterinary drug residues in shrimp: a multi-class method by liquid chromatography-quadrupole ion trap mass spectrometry.

    PubMed

    Li, Hui; Kijak, Philip James; Turnipseed, Sherri B; Cui, Wei

    2006-05-19

    A liquid chromatography-mass spectrometry (LC-MS) method was developed to screen and confirm veterinary drug residues in raw shrimp meat. This method simultaneously monitors 18 drugs of different classes, including oxytetracycline (OTC), sulfonamides, quinolones, cationic dyes, and toltrazuril sulfone (TOLS). The homogenized shrimp meat is extracted with 5% trichloroacetic acid. The extract is further cleaned using polymer-based SPE. A 50 mm phenyl column separates the analytes, prior to analysis with an ion trap mass spectrometer interfaced with an atmospheric pressure chemical ionization source. This method is able to confirm oxytetracycline residues at 200 ng/g, toltrazuril sulfone at 50 ng/g, sulfaquinoxaline at 20 ng/g, and the other 15 drugs at 10 ng/g or lower levels. An estimate of the level of residues can also be made so that only confirmed samples above action levels will be sent for quantitation. The method is validated with both fortified and incurred samples, using multiple shrimp species as well. This multi-class method can provide a means to simultaneously monitor for a wide range of illegal drug residues in shrimp. PMID:16597519

  3. Qualitative and quantitative characterization of phenolic and diterpenoid constituents in Danshen (Salvia miltiorrhiza) by comprehensive two-dimensional liquid chromatography coupled with hybrid linear ion trap Orbitrap mass.

    PubMed

    Cao, Ji-Liang; Wei, Jin-Chao; Hu, Yuan-Jia; He, Cheng-Wei; Chen, Mei-Wan; Wan, Jian-Bo; Li, Peng

    2016-01-01

    Danshen is one of the most frequently used traditional Chinese herbs owing to its remarkable and reliable therapeutic effects. Phenolic acids and diterpenoids have proved to be the bioactive substance groups. In order to fully profile its chemical compositions and explore new potential bioactive compounds, a comprehensive two-dimensional liquid chromatography system coupled to DAD detector and hybrid linear ion trap (LTQ) Orbitrap mass spectrometry (LC × LC-DAD-ESI/HRMS/MS(n)) was set up in this study based on the column combination of Hypersil gold CN (150 mm × 1 mm, 3 μm) and Accucore C18 (50 mm × 4.6 mm, 2.6 μm). Using the optimal segment gradient program, phenolic acids and diterpenoids were separated into two independent groups and a total of 328 peaks were successfully detected on the contour plot of Danshen. By means of the accurate mass and reliable MS(n) data, 102 compounds were identified or tentatively identified and 7 of them were discovered from Danshen for the first time. Moreover, the LC × LC-DAD system was validated for the quantitative analysis of 14 bioactive analytes using the contour plot, exhibiting satisfactory linearity (r ≥ 0.9976) and high precision for both peak locating (≤ 1.07%) and peak volume calculating (0.34%-4.11%). The established method could afford powerful separation capability, reliable identification data and accurate quantitative results, which is very suitable for analysis of complex herbal samples. PMID:26687169

  4. Studies on the metabolism of mitragynine, the main alkaloid of the herbal drug Kratom, in rat and human urine using liquid chromatography-linear ion trap mass spectrometry.

    PubMed

    Philipp, Anika A; Wissenbach, Dirk K; Zoerntlein, Siegfried W; Klein, Oliver N; Kanogsunthornrat, Jidapha; Maurer, Hans H

    2009-08-01

    Mitragynine (MG) is an indole alkaloid of the Thai medicinal plant Mitragyna speciosa (Kratom in Thai) and reported to have opioid agonistic properties. Because of its stimulant and euphoric effects, Kratom is used as a herbal drug of abuse. The aim of the presented study is to identify the phase I and II metabolites of MG in rat and human urine after solid-phase extraction (SPE) using liquid chromatography-linear ion trap mass spectrometry providing detailed structure information in the MSn mode particularly with high resolution. The seven identified phase I metabolites indicated that MG was metabolized by hydrolysis of the methylester in position 16, O-demethylation of the 9-methoxy group and of the 17-methoxy group, followed, via the intermediate aldehydes, by oxidation to carboxylic acids or reduction to alcohols and combinations of some steps. In rats, four metabolites were additionally conjugated to glucuronides and one to sulfate, but in humans, three metabolites to glucuronides and three to sulfates. PMID:19536806

  5. Quantitative determination of isoquinoline alkaloids and chlorogenic acid in Berberis species using ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry.

    PubMed

    Singh, Awantika; Bajpai, Vikas; Kumar, Sunil; Arya, Kamal Ram; Sharma, Kulwant Rai; Kumar, Brijesh

    2015-06-01

    Berberis species are well known and used extensively as medicinal plants in traditional medicine. They have many medicinal values attributable to the presence of alkaloids having different pharmacological activities. In this study, a method was developed and validated as per international conference on harmonization guidelines using ultra high performance liquid chromatography with hybrid triple quadrupole-linear ion trap mass spectrometry operated in the multiple reaction monitoring mode for nine bioactive compounds, including protoberberine alkaloids, aporphine alkaloids and chlorogenic acid. This method was applied in different plant parts of eight Berberis species to determine variations in content of nine bioactive compounds. The separation was achieved on an ACQUITY UPLC CSH™ C18 column using a gradient mobile phase at flow rate 0.3 mL/min. Calibration curves for all the nine analytes provided optimum linear detector response (with R(2) ≥0.9989) over the concentration range of 0.5-1000 ng/mL. The precision and accuracy were within RSDs ≤2.4 and ≤2.3%, respectively. The results indicated significant variation in the total contents of the nine compounds in Berberis species. PMID:25847792

  6. Simultaneous determination of plant hormones in peach based on dispersive liquid-liquid microextraction coupled with liquid chromatography-ion trap mass spectrometry.

    PubMed

    Lu, Qiaomei; Zhang, Wenmin; Gao, Jia; Lu, Minghua; Zhang, Lan; Li, Jianrong

    2015-06-15

    Fruit development is influenced greatly by endogenous hormones including salicylic acid (SA) and abscisic acid (ABA). Mass spectrometry with high sensitivity has become a routine technology to analyze hormones. However, pretreatment of plant samples remains a difficult problem. Thus, dispersive liquid-liquid microextraction (DLLME) was used to concentrate trace plant hormones before liquid chromatography-ion trap mass spectrometry (LC-ITMS) analysis. Standard curves were linear within the ranges of 0.5-50, 0.2-20ng/mL for SA and ABA, respectively. The correlation coefficients were greater than 0.9995 with recoveries above 87.5%. The limits of detection were 0.2ng/mL for SA and 0.1ng/mL for ABA in spiked water solution, respectively (injection 20μL). The successful analysis of SA and ABA in fruit samples indicated our DLLME-LC-ITMS approach was efficient, allowing reliable quantification of both two compounds from very small amounts of plant material. Moreover, this research revealed the relationship between SA and ABA content and development of peach fruit at different growth stages. PMID:25939092

  7. [Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].

    PubMed

    Li, Zhaoyong; Wang, Fengmei; Niu, Zengyuan; Luo, Xin; Zhang, Gang; Chen, Junhui

    2014-05-01

    A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) using a gradient elution of acetonitrile/water containing 0.1% (v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3 x 10(-6) (3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N = 3) of the 24 compounds were < or = 10 microg/kg, which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics. PMID:25185307

  8. Determination of carnitine and acylcarnitines in plasma by high-performance liquid chromatography/electrospray ionization ion trap tandem mass spectrometry.

    PubMed

    Vernez, Laurence; Wenk, Markus; Krähenbühl, Stephan

    2004-01-01

    A high-performance liquid chromatography/mass spectrometry method was developed for the determination of carnitine, its biosynthetic precursor butyrobetaine, and eight acylcarnitines in plasma. The procedure includes a solid-phase extraction for carnitine and short- and medium-chain acylcarnitines, and a liquid-liquid extraction for protein-bound long-chain acylcarnitines, followed by separation on a reversed-phase column in the presence of a volatile ion-pairing reagent. Detection was achieved using an ion-trap mass spectrometer run in the tandem mass spectrometry (MS/MS) mode. The choice of the matrix for calibrators, used for quantification of these endogenous compounds, was also investigated. Validation was performed for standard quality controls diluted with 4% bovine serum albumin solution and for spiked plasma quality control samples at concentrations between 0.5 and 80 micromol/L, depending on the compound. Intra- and inter-day precisions for the determination of carnitine were below 3.4% and accuracies were between 95.2 and 109.0%. Application of the method to the diagnosis of pathological acylcarnitine profiles of metabolic disorders in a patient suffering from methylmalonic aciduria is presented. The method allows quantification of carnitine, butyrobetaine, acetylcarnitine and propionylcarnitine, and semiquantitative analysis of medium- and long-chain acylcarnitines. In contrast with other methods, no derivatization step is needed. PMID:15164354

  9. Validation of a new liquid chromatography- tandem mass spectrometry ion-trap technique for the simultaneous determination of thirteen anticoagulant rodenticides, drugs, or natural products.

    PubMed

    Fourel, Isabelle; Hugnet, Christophe; Goy-Thollot, Isabelle; Berny, Philippe

    2010-03-01

    The purpose of this study was to develop and validate a liquid chromatography-tandem mass spectrometry method for the identification and quantification of anticoagulant (anti-vitamin K or AVK) compounds, including rodenticides, drugs, and natural products because no published method could be found. The proposed method is based on ion-trap technology with electrospray ionization (ESI) and multiple reaction monitoring (MRM) technique. Each AVK is identified by means of its retention time, precursor ion, and two product ions. Plasma samples are extracted by liquid-liquid partition on Toxi-tube B((R)). The method was validated on dog plasma and gave good results in terms of specificity, linearity, and percent recovery for the 14 AVK tested (warfarin, acenocoumarol, bromadiolone, brodifacoum, chlorophacinone, coumatetralyl, dicoumarol, difenacoum, difethialone, flocoumafen, fluindione, phenindione, and tioclomarol). The limits of detection ranged from 5 to 25 ng/mL. Intraday repeatability was good, but interday repeatability was more variable though still sufficient for our diagnostic purposes. The technique was successfully applied in a series of clinical investigations to demonstrate its applicability in various animal species and gave very high sensitivity and specificity results. PMID:20223102

  10. Detection and chemical profiling of Ling-Gui-Zhu-Gan decoction by ultra performance liquid chromatography-hybrid linear ion trap-Orbitrap mass spectrometry.

    PubMed

    Wang, Pei; Wang, Bo; Xu, Jingyao; Sun, Jianbo; Yan, Qin; Ji, Bin; Zhao, Yunli; Yu, Zhiguo

    2015-02-01

    Ling-Gui-Zhu-Gan decoction (LGZGD), a well-known traditional Chinese medicine (TCM) formula, has been extensively used for the treatment of cardiovascular disease in clinic. However, the chemical constituents in LGZGD had not been investigated so far. In this study, an ultra performance liquid chromatography-hybrid electrospray ionization linear ion trap-Orbitrap mass spectrometry (UPLC-LTQ-Oribitrap-MS/MS) method was established for rapid separation and structural identification of the constituents in LGZGD. Separation was performed on an ACQUITY(TM) UPLC BEH C18 column (50 × 2.1 mm, 1.7 μm) by gradient elution mode, using acetonitrile-water containing 0.1% formic acid as mobile phase at the flow rate of 0.2 mL/min. Accurate mass measurement for molecular ions and characteristic fragment ions could represent identification criteria for these compounds. As a result, 95 compounds including triterpene acids, triterpene saponins, flavonoids, coumarins, coumestans, benzofurans, phenylpropanoids and sesquiterpenoid lactones were detected, and 90 of them were tentatively identified. All compounds were further assigned in the individual raw material. In conclusion, the UPLC-LTQ-Orbitrap-MS/MS is a highly efficient technique to separate and identify constituents in complex matrices of TCMs. These results obtained in this research will provide a basis for quality control and further in vivo study of LGZGD. PMID:24920655

  11. Determination of non-ionic polyethoxylated surfactants in sewage sludge by coacervative extraction and ion trap liquid chromatography-mass spectrometry.

    PubMed

    Cantero, Manuel; Rubio, Soledad; Pérez-Bendito, Dolores

    2004-08-13

    Alkylphenol polyethoxylates (APE, nonyl and octyl) and alcohol ethoxylates (AE, C12-C16) were analysed in sewage sludge by extraction with sodium dodecane sulphonate (SDoS), that undergoes coacervation under acid conditions, followed by quantitation with liquid chromatography/atmospheric pressure chemical ionisation ion/trap mass spectrometry, in positive ion mode. Coacervative extraction was optimised using an aged, fortified dehydrated sludge. Recoveries ranged from 78 to nearly 100% irrespective of the sludge matrix analysed. The method provided good agreement between the ethoxamer distribution of surfactants after extraction from sludge and that in the original surfactant. Detection limits for polyethoxylated surfactants in the sludge were 0.09-0.38 mg/kg. The procedure was used to assess the concentrations of APE and AE in activated and dehydrated sludge from two sewage treatment plants. Polyethoxylates were found in all samples in the concentration ranges 11-151, 100-138 and 23-141 mg/kg for octylphenol, nonylphenol and individual AE homologues, respectively. The method did not require clean-up or preconcentration steps. PMID:15387183

  12. Determination of alkylphenols and alkylphenol carboxylates in wastewater and river samples by hemimicelle-based extraction and liquid chromatography-ion trap mass spectrometry.

    PubMed

    Cantero, Manuel; Rubio, Soledad; Pérez-Bendito, Dolores

    2006-07-01

    Sodium dodecyl sulfate (SDS)-coated alumina and cetylpyridinium chloride (CPC)-coated silica were investigated as new sorbents for the concentration of alkylphenol polyethoxylate (APE) biodegradation products from wastewater and river water samples. Octylphenol (OP), nonylphenol (NP), octylphenol carboxylic acid (OPC) and nonylphenol carboxylic acid (NPC) were quantitatively retained on both supramolecular sorbents on the basis of the formation of mixed hemimicelles and admicelles. SDS hemimicelles-based SPE was proposed for the extraction/concentration of the target compounds prior to their separation and quantitation by liquid chromatography/electrospray ionization in negative mode, ion trap mass spectrometry. No clean-up steps or evaporation of the eluent were required. The recovery of APE metabolites from sewage and river water ranged between 87 and 100%. Concentration factors of about 500, using sample volumes of 1 l, were achieved. Detection limits were between 75 and 193 ng/l. The approach developed was applied to the determination of alklylphenols and alkylphenol carboxylic acids in raw and treated sewage and river samples. The concentrations of APE metabolites found ranged between 0.8 and 78 microg/l. PMID:16412449

  13. Quantitative and qualitative profiling of endocannabinoids in human plasma using a triple quadrupole linear ion trap mass spectrometer with liquid chromatography.

    PubMed

    Thomas, Aurélien; Hopfgartner, Gérard; Giroud, Christian; Staub, Christian

    2009-03-01

    Owing to the large implication of endocannabinoids (ECs) in many physiological and pathophysiological processes, a rapid liquid chromatography/electrospray ionisation triple quadrupole linear ion trap mass spectrometric assay (LC/ESI-QqQ(LIT)) was developed for the detection and characterization of anandamide (AEA), 2-arachidonoyl glycerol (2-AG), virodhamine (VA), noladin ether (2-AGE), and N-arachidonoyl dopamine (NADA) in human plasma. The ECs were extracted from 500 microL of plasma by liquid-liquid extraction (LLE) and separated by using an XTerra C18 MS column (50 x 3.0 mm i.d., 3.5 microm) with gradient elution. The mobile phase was composed of a mixture of acetonitrile, water, and formic acid (0.1%). For confirmatory analysis, an information-dependent acquisition (IDA) experiment was performed with selected reaction monitoring (SRM) as survey scan and enhanced product ion (EPI) as dependent scan. The assay was found to be linear in the concentration range of 0.1-5 ng/mL for AEA, 0.3-5 ng/mL for VA, 2-AGE, and NADA and 1-20 ng/mL for 2-AG using a 0.5 mL aliquot of plasma. Repeatability and intermediate precision were found less than 15% over the tested concentration ranges. The developed method thus provided the rapid, highly sensitive and highly selective requirement for assess quantitation, and identification of ECs in plasma. PMID:19170046

  14. Polar organic chemical integrative sampling and liquid chromatography- electrospray/ion-trap mass spectrometry for assessing selected prescription and illicit drugs in treated sewage effluents

    USGS Publications Warehouse

    Jones-Lepp, T. L.; Alvarez, D.A.; Petty, J.D.; Huckins, J.N.

    2004-01-01

    The purpose of the research presented in this paper was twofold: (1) to demonstrate the coupling of two state-of-the-art techniques: a time-weighted polar organic chemical integrative sampler (POCIS) and microliquid chromatography-electrospray/ion-trap mass spectrometry and (2) to assess the ability of these methodologies to detect six drugs (azithromycin, fluoxetine, omeprazole, levothyroxine, methamphetamine, methylenedioxymethamphetamine [MDMA]) in a real-world environment, e.g., waste water effluent. In the effluent from three wastewater treatment plants (WWTPs), azithromycin was detected at concentrations ranging from 15 to 66 ng/L, which is equivalent to a total annual release of 1 to 4 kg into receiving waters. Detected and confirmed in the effluent from two WWTPs were two illicit drugs, methamphetamine and MDMA, at 2 and 0.5 ng/L, respectively. Although the ecotoxicologic significance of drugs in environmental matrices, particularly water, has not been closely examined, it can only be surmised that these substances have the potential to adversely affect biota that are continuously exposed to them even at very low levels. The potential for chronic effects on human health is also unknown but of increasing concern because of the multi-use character of water, particularly in densely populated, arid areas.

  15. An integrated strategy to quantitatively differentiate chemome between Cistanche deserticola and C. tubulosa using high performance liquid chromatography-hybrid triple quadrupole-linear ion trap mass spectrometry.

    PubMed

    Song, Yuelin; Song, Qingqing; Li, Jun; Zhang, Na; Zhao, Yunfang; Liu, Xiao; Jiang, Yong; Tu, Pengfei

    2016-01-15

    It is important to conduct large-scale detection, identification, and quantitation of metabolites in a given sample. Herein, a practical strategy was proposed to quantitatively compare the chemome between Cistanche deserticola (CD) and C. tubulosa (CT), which have been widely believed as the ideal edible and medicinal plants for conquering the deserts. The entire workflow was implemented on high performance liquid chromatography-hybrid triple quadrupole-linear ion trap mass spectrometer and consisted of three primary steps: (1) component detection and identification, various mass spectrometric approaches were applied to globally screen the chemical constituents, and structural elucidation was achieved by comparing with authentic compounds, analyzing MS(2) spectra, and referring to the literature along with accessible databases; (2) comprehensive relative quantitation, scheduled multiple reaction monitoring algorithm was introduced for relative quantitation of all detected ingredients; and (3) chemome comparison, the quantitative dataset was subjected for multivariate statistical analysis to carry out comparative study. A total of 513 metabolites were detected and relatively quantitated, and 379 ones were annotated. Betaine, Krebs cycle intermediates, phenylethanoid glycosides, and iridoids were picked out as the chemical markers being responsible for the discrimination of the chemical profiles between CD and CT. Above all, the quantitative chemome of CD and CT were exhaustively characterized and compared, which could advance their values concerning drug development, economics, and desertification control. The proposed strategy is expected as a reliable choice for widely targeted metabolomics of plants. PMID:26742897

  16. Analysis and comparison of glucocerebroside species from three edible sea cucumbers using liquid chromatography-ion trap-time-of-flight mass spectrometry.

    PubMed

    Xu, Jie; Duan, Jingjing; Xue, Changhu; Feng, Tingyu; Dong, Ping; Sugawara, Tatsuya; Hirata, Takashi

    2011-11-23

    Sphingolipids constitute a highly diverse and complex class of molecules and exhibit important physiological functions. Glucocerebrosides are anticipated to play a positive role in human nutrition. In this study, complicated glucocerebrosides from three specimens of edible sea cucumbers, specifically, Acaudina molpadioides, Cucumaria frondosa, and Apostichopus japonicus, were rapidly identified using liquid chromatography-ion trap-time-of-flight mass spectrometry (LCMS-IT-TOF), which is a powerful analysis tool. [M + H](+), [M + Na](+), and [M + H - H(2)O](+) in positive electrospray ionization (ESI) mode were used for MS/MS analysis to obtain product ion spectra. Various long-chain bases of glucocerebrosides were found in these sea cucumbers. Two of the most common long-chain bases were 2-amino-1,3-dihydroxy-4-heptadecene (d17:1) and 4,8-sphingadienine (d18:2), which were acylated to form saturated and monounsaturated nonhydroxy and monohydroxy fatty acids with 18-25 carbon atoms. The glucocerebroside molecular species were the most complicated in the sea cucumber C. frondosa and were the simplest in the sea cucumber A. molpadioides. PMID:22004409

  17. Liquid chromatography quadrupole linear ion trap mass spectrometry for quantitative steroid hormone analysis in plasma, urine, saliva and hair.

    PubMed

    Gaudl, Alexander; Kratzsch, Juergen; Bae, Yoon Ju; Kiess, Wieland; Thiery, Joachim; Ceglarek, Uta

    2016-09-16

    Steroid analysis is being conquered by liquid chromatography tandem mass spectrometry (LC-MS/MS) benefiting from higher standardization, selectivity and diversity. Regarding high throughput in routine diagnostics rapid chromatography is mandatory. Introducing MS(3) (MS/MS/MS), specificity of mass spectrometric detection can be enhanced without sacrificing analysis time. 100mL of human plasma/serum, saliva, urine and 10-20mg of hair are used for the simultaneous quantification of 17α-hydroxyprogesterone, aldosterone, androstenedione, cortisol, cortisone, dehydroepiandrosterone sulfate (DHEAS), estradiol, progesterone, and testosterone using online solid phase extraction (SPE) LC-MS/MS or LC-MS(3). Steroids can be analyzed in 4min after a single manual dilution and protein precipitation step. In complex sample matrices like hair MS(3) detection was found to be appropriate for quantitation. Lower limits of quantitation ranged from 37pmol/L (estradiol) up to 3.1nmol/L (DHEAS). General accuracy was 89-107% with between-run imprecision ≤10%. Comparison to immunoassays revealed significant differences in quantitation for urinary cortisol (-71% mean), aldosterone (-40% mean) and plasma aldosterone (-45% mean). The comparison of MS(2) and MS(3) quantitation of hair cortisol also revealed significant differences. In general, quantitation via MS(3) was not applicable for a long time. But with the current generation of mass spectrometers quantitation via MS(3) can be superior to MS(2) regarding specificity and accuracy when dealing with matrix issues. However, drawbacks regarding flexibility and precision have to be taken into account. Concludingly, simple protein precipitation combined with rapid online SPE LC-MS/MS/MS allows us to quantify over broad, essential concentration ranges in human serum, saliva, urine and hair. PMID:27554022

  18. Asymmetric ion trap

    DOEpatents

    Barlow, Stephan E.; Alexander, Michael L.; Follansbee, James C.

    1997-01-01

    An ion trap having two end cap electrodes disposed asymmetrically about a center of a ring electrode. The inner surface of the end cap electrodes are conformed to an asymmetric pair of equipotential lines of the harmonic formed by the application of voltages to the electrodes. The asymmetry of the end cap electrodes allows ejection of charged species through the closer of the two electrodes which in turn allows for simultaneously detecting anions and cations expelled from the ion trap through the use of two detectors charged with opposite polarity.

  19. [Identification of banned aromatic amines and their isomers in textiles by ultra-performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].

    PubMed

    Ye, Xiwen; Peng, Yan; Niu, Zengyuan; Gao, Yonggang; Luo, Xin; Zou, Li; Zhou, Minghui

    2014-09-01

    A method of ultra-performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was used to screen and confirm 24 banned aromatic amines and their 14 isomers at the same time. The main factors influencing the separation including the column, and the nature of make-up solvent were optimized. Under the optimized experimental conditions, the analytes were reduced to banned aromatic amine with sodium dithionite, extracted by methyl tert-butyl ether and loaded onto a ZORBAX SB-C18 column (150 mm x 2.1 mm, 5 μm) with a gradient elution of methanol and 0.1% formic acid aqueous solution, and finally detected by LTQ/Orbitrap MS. The screening and quantitative analysis were carried out by the accurate mass of quasi-molecular ion and the peak in extracted chromatogram with accurate mass. The correlation coefficients were higher than 0.99 and the limits of detection were in the range of 0.5-5 μg/kg. The method could screen and confirm the 24 banned aromatic amines and their 14 isomers at the same time. The results were 1.56 mg/kg of 4-chloroaniline, 0.34 mg/kg of o-toluidine, and 0.81 mg/kg of 2,6-toluylenediamine with the relative standard deviations ranging from 0.27% to 1.32% in actual samples. The results indicate that the developed method is simple, efficient and precise, and can be a reliable technique for the separation of the 24 banned aromatic amines and their 14 isomers in textile samples. PMID:25752096

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

    PubMed

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

    2000-01-01

    This work describes a new method for the quantitation of trace amounts of sulfamethazine (SMZ) and its main metabolite, N4-acetylsulfamethazine (Ac-SMZ), in swine urine, using high-performance liquid chromatography (HPLC) tandem mass spectrometric analysis of crude urine after addition of internal standard and simple dilution with water. The aim was to determine whether residues of this sulfamidic drug, normally administered to swine in order to prevent infectious diseases, were present in urine at levels lower than those permitted by regulatory authorities before human consumption (EU Project SMT, contract number CT 96-2092). A 10 microL volume of diluted urine was injected into a very short, narrow-bore chromatographic column (Zorbax SB-C18 2.1 i. d. x30 mm length, 3.5 microm pore size). Elution of the analytes of interest was achieved in less than seven minutes using a rapid gradient (from 20 to 80% methanol in 3 minutes). Either a PE Sciex API 365 triple quadrupole (QqQ), operated in the selected reaction monitoring (SRM) mode, or a Finnigan LCQ ion trap (IT) mass spectrometer, operated in narrow-range product ion scan, was used as the final detector. Electrospray (ESI) was used as the ionization technique. A comparison of the two tandem mass spectrometers was performed by analyzing the same set of test samples, at three concentration levels, on three different days. Linearity of responses of the calibration standards, intra- and inter-assay precision of the samples, specificity and limits of detection were evaluated for both systems. Both the QqQ and the IT instrument was suitable for rapid, sensitive and specific determination of the analytes, although the overall performance of the QqQ was slightly superior in terms of linearity, precision and sensitivity. PMID:10844733

  1. Multi-residue method for trace level determination of pharmaceuticals in solid samples using pressurized liquid extraction followed by liquid chromatography/quadrupole-linear ion trap mass spectrometry.

    PubMed

    Jelić, Aleksandra; Petrović, Mira; Barceló, Damià

    2009-11-15

    A simple and sensitive method for simultaneous analysis of 43 pharmaceutical compounds in sewage sludge and sediment samples was developed and validated. The target compounds were extracted using pressurized liquid extraction (PLE) and then purified and pre-concentrated by solid phase extraction (SPE) using a hydrophilic-lipophilic balanced polymer. PLE extraction was performed on temperature of 100 degrees C, with methanol/water mixture (1/2, v/v) as extraction solvent. The quantitative analysis was performed by liquid chromatography tandem mass spectrometry using a hybrid triple quadrupole-linear ion trap mass spectrometer (LC-QqLIT-MS). Data acquisition was carried out in selected reaction monitoring (SRM) mode, monitoring two SRM transitions to ensure an accurate identification of target compounds in the samples. Additional identification and confirmation of target compounds were performed using the Information Dependent Acquisition (IDA) function. The method was validated through the estimation of the linearity, sensitivity, repeatability, reproducibility and matrix effects. The internal standard approach was used for quantification because it efficiently corrected matrix effects. Despite the strong matrix interferences, the recoveries were generally higher of 50% in both matrixes and the detection and quantification limits were very low. Beside the very good sensitivity provided by LC-QqLIT-MS, an important characteristic of the method is that all the target compounds can be simultaneously extracted, treated and analysed. Hence, it can be used for routine analysis of pharmaceuticals providing large amount of data. The method was applied for the analysis of pharmaceuticals in river sediment and wastewater sludge from three treatment plants with different treatment properties (i.e. capacity, secondary treatment, quality of influent waters). The analysis showed a widespread occurrence of pharmaceuticals in the sludge matrices. PMID:19782237

  2. Quantitative determination of capsaicin, a transient receptor potential channel vanilloid 1 agonist, by liquid chromatography quadrupole ion trap mass spectrometry: evaluation of in vitro metabolic stability.

    PubMed

    Beaudry, Francis; Vachon, Pascal

    2009-02-01

    Capsaicin is the most abundant pungent molecule present in red peppers and it is widely used for food flavoring, in pepper spray in self-defense devices and more recently in ointments for the relief of neuropathic pain. Capsaicin is a selective agonist of transient receptor potential channel, vanilloid subfamily member 1. A selective and sensitive quantitative method for the determination of capsaicin by LC-ESI/MS/MS was developed. The method consisted of a protein precipitation extraction followed by analysis using liquid chromatography electrospray quadrupole ion trap mass spectrometry. The chromatographic separation was achieved using a 100 x 2 mm C(18) Waters Symmetry column combined with a gradient mobile phase composed of acetonitrile and 0.1% formic acid aqueous solution at a flow rate of 220 microL/min. The mass spectrometer was operating in full-scan MS/MS mode using two-segment analysis. An analytical range of 10-5000 ng/mL was used in the calibration curve constructed in rat plasma. The interbatch precision and accuracy observed were 6.5, 6.7, 5.3 and 101.2, 102.7, 103.5% at 50, 500 and 5000 ng/mL, respectively. An in vitro metabolic stability study was performed in rat, dog and mouse liver microsomes and the novel analytical method was adapted and used to determine intrinsic clearance of capsaicin. Results suggest very rapid degradation with T(1/2) ranging from 2.3 to 4.1 min and high clearance values suggesting that drug bioavailability will be considerably reduced, consequently affecting drug response and efficacy. PMID:18816461

  3. Use of liquid chromatography-atmospheric pressure chemical ionization-ion trap mass spectrometry for identification of oleanolic acid and ursolic acid in Anoectochilus roxburghii (wall.) Lindl.

    PubMed

    Huang, Liying; Chen, Tianwen; Ye, Zhao; Chen, Guonan

    2007-07-01

    Oleanolic acid (OA) and ursolic acid (UA) are the two important bioactive compounds in Anoectochilus roxburghii (wall) Lindl (A. roxburghii), which has been used as a traditional Chinese medicine. So far, there has been no report to indicate that A. roxburghii contains these two bioactive compounds. It is necessary to develop an effective method to extract and analyze OA and UA in A. roxburghii. In this paper, a quantitative method, consisting of supercritical fluid extraction (SFE) followed by liquid chromatography-atmospheric pressure chemical ionization-ion trap mass spectrometry (LC-APCI-IT-MS) analysis, was developed for identification of OA and UA in A. roxburghii. The extraction was carried out by using CO(2) as the supercritical fluid and ethanol as the modifier before LC separation. The mobile phase used for LC separation consisted of acetic acid (1%, v/v), water (15%, v/v) and methanol (84%, v/v), and the elution was performed at a flow rate of 0.8 ml/min. The mass spectrometer was operated in APCI(+) mode with selected ion monitoring (SIM) to quantify OA and UA at m/z 439.4. Under optimum conditions, the linear responses of OA and UA were obtained in the concentration range of 0.5-80 (r = 0.9992) and 0.5-50 microg/ml (r = 0.9989) with the detection limits of 0.125 and 0.085 microg/ml, respectively. The proposed method has been used for the identification and quantitation of OA and UA in a real A. roxburghii sample. PMID:17535010

  4. Simultaneous determination of diclofenac, its human metabolites and microbial nitration/nitrosation transformation products in wastewaters by liquid chromatography/quadrupole-linear ion trap mass spectrometry.

    PubMed

    Osorio, Victoria; Imbert-Bouchard, Marta; Zonja, Bozo; Abad, José-Luis; Pérez, Sandra; Barceló, Damià

    2014-06-20

    An analytical method was developed and validated for the first determination of five major human metabolites of the non-steroidal anti-inflammatory drug diclofenac as well as two microbial transformation products in wastewater. The method was based on the extraction of diclofenac and the chemically synthetized compounds by solid-phase extraction (SPE), using a hydrophilic-lipophilic balanced polymer followed by liquid chromatography (LC) coupled to hybrid quadrupole-linear ion trap mass spectrometry (QqLIT-MS). Quantitation was performed by the internal standard approach, to correct for matrix effects. The accuracy of the method was generally higher than 40% for raw and treated wastewater with a precision below 12%. In wastewater influent and effluent samples the detection limits for the majority of target compounds were 0.3-2.5ngL(-1) and 0.1-3.1ngL(-1), respectively. The method was applied to the analysis of influent and effluent wastewater samples from urban wastewater treatment plants. Moreover, to obtain an extra tool for confirmation and identification of the studied diclofenac-derived compounds, Information-Dependent Acquisition (IDA) experiments were performed, with selected reaction monitoring (SRM) as the survey scan and an enhanced product ion (EPI) scan as the dependent scan. Diclofenac and its major human metabolite, 4'-hydroxydiclofenac were detected in all samples at concentrations of 331-1150ngL(-1) and 585-6000ngL(-1), respectively. Neither microbial transformation product of diclofenac was detected in any of the influent samples analyzed, but in effluents, their concentrations ranged from 4 to 105ngL(-1). PMID:24835592

  5. Highly sensitive simultaneous determination of sulfonamide antibiotics and one metabolite in environmental waters by liquid chromatography-quadrupole linear ion trap-mass spectrometry.

    PubMed

    Díaz-Cruz, M Silvia; García-Galán, M Jesús; Barceló, Damià

    2008-06-01

    The present work describes the development of a highly sensitive analytical method based on liquid chromatography-quadrupole linear ion trap-mass spectrometry (LC-QqLIT-MS) for the determination of nine sulfonamide antibiotics and one N4-acetylated metabolite in environmental waters (wastewater, surface water and groundwater) and bottled mineral water. Special emphasis was devoted to the elimination of matrix components during solid-phase extraction (SPE) by the evaluation of three different extraction/purification strategies: single cartridges (Oasis HLB and Oasis MCX) and tandem (TD) extraction (combination of both). The method developed proved to be suitable for sulfonamide determination in all kinds of waters tested. The method was shown to be linear in a wide concentration range, with correlation coefficients higher than 0.999 for all compounds except for sulfadimethoxine (R2 0.997). The overall instrumental repeatability was satisfactory, with the exception of the metabolite (RSD 34%). Method limits of detection achieved for sulfonamides were in the range 0.01-1.13 ng L(-1) and for the metabolite 0.08-461 ng L(-1). Recovery rates were estimated at 500 ng L(-1) spike level in the four water matrices selected. The highest recovery achieved in all matrices was that corresponding to the Oasis HLB cartridge. In environmental waters, recovery values obtained were higher than 61% for the surface water and, in general, higher than 90% for groundwater and wastewater. Bottled mineral water exhibited recovery rates higher than 92%, with the exception of sulfamethoxypiridazine (82%) and sulfapyridine (86%) In order to demonstrate the applicability of the developed method, several water samples were analyzed. Results evidenced the requirement for consideration of N4-acetylated metabolites of sulfonamides in environmental residue analysis to avoid the underestimation of removal rates of such pharmaceutical compounds during wastewater treatments. PMID:18440009

  6. [Rapid screening and identification of 22 allergenic disperse dyes in ecological textiles by high performance liquid chromatography-linear ion trap/orbitrap mass spectrometry].

    PubMed

    Niu, Zengyuan; Luo, Xin; Ye, Xiwen; Xiu, Xiaoli; Zhang, Li; Wang, Xin; Chen, Jing

    2015-10-01

    A rapid screening method based on high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry (HPLC-LTQ/Orbitrap MS) for 22 disperse dyes in ecological textiles has been established. The target compounds were extracted by pyridine/water (1:1, v/v) by shaking extraction in 90 degrees C water bath. The extracts were then separated by a CAPCELL PAK C18 column (100 mm x 2.0 mm, 5 μm) using gradient elution with acetonitrile-5 mmol/L ammonium acetate containing 0.01% (v/v) formic acid as mobile phases, and finally analyzed by HPLC-LTQ/Orbitrap in positive and negative ESI modes. The retention time and accurate mass of parent ion were used for fast screening of 22 disperse dyes, while the confirmatory analysis was obtained by fragments generated by collision-induced dissociation (CID) MS/MS. Target analysis exhibited high mass accuracy (< 5 x 10(-6)). Each target showed a good linearity in its own concentration range and the correlation coefficient was higher than 0.99. The LOQs were 0.125-2.5 mg/kg. Except for Disperse Yellow 49, the average recoveries of most disperse dyes at three spiked levels were 65%-120%, and the relative standard deviations (n = 6) were less than 15%. The method was applied for screening 40 different kinds of textiles, and Disperse Orange 37/76 was detected in one of them. With high selectivity and strong anti-jamming ability, this method is simple, rapid, accurate, and it can be used for the inspection of disperse dyes in textiles. PMID:26930969

  7. Characterizing the gas phase ion chemistry of an ion trap mobility spectrometry based explosive trace detector using a tandem mass spectrometer.

    PubMed

    Kozole, Joseph; Tomlinson-Phillips, Jill; Stairs, Jason R; Harper, Jason D; Lukow, Stefan R; Lareau, Richard T; Boudries, Hacene; Lai, Hanh; Brauer, Carolyn S

    2012-09-15

    A commercial-off-the-shelf (COTS) ion trap mobility spectrometry (ITMS) based explosive trace detector (ETD) has been interfaced to a triple quadrupole mass spectrometer (MS/MS) for the purpose of characterizing the gas phase ion chemistry intrinsic to the ITMS instrument. The overall objective of the research is to develop a fundamental understanding of the gas phase ionization processes in the ITMS based ETD to facilitate the advancement of its operational effectiveness as well as guide the development of next generation ETDs. Product ion masses, daughter ion masses, and reduced mobility values measured by the ITMS/MS/MS configuration for a suite of nitro, nitrate, and peroxide containing explosives are reported. Molecular formulas, molecular structures, and ionization pathways for the various product ions are inferred using the mass and mobility data in conjunction with density functional theory. The predominant product ions are identified as follows: [TNT-H](-) for trinitrotoluene (TNT), [RDX+Cl](-) for cyclo-1,3,5-trimethylene-2,4,6-trinitramine (RDX), [NO(3)](-) for ethylene glycol dinitrate (EGDN), [NG+NO(3)](-) for nitroglycerine (NG), [PETN+NO(3)](-) for pentaerythritol tetranitrate (PETN), [HNO(3)+NO(3)](-) for ammonium nitrate (NH(4)NO(3)), [HMTD-NC(3)H(6)O(3)+H+Cl](-) for hexamethylene triperoxide diamine (HMTD), and [(CH(3))(2)CNH(2)](+) for triacetone triperoxide (TATP). The predominant ionization pathways for the formation of the various product ions are determined to include proton abstraction, ion-molecule attachment, autoionization, first-order and multi-order thermolysis, and nucleophilic substitution. The ion trapping scheme in the reaction region of the ITMS instrument is shown to increase predominant ion intensities relative to the secondary ion intensities when compared to non-ion trap operation. PMID:22967626

  8. Gas chromatography in space

    NASA Technical Reports Server (NTRS)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  9. [Simultaneous determination of nine beta-blockers in porcine tissues by ultra-fast liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry].

    PubMed

    Zhang, Hongwei; Xu, Hui; Gao, Jianguo; Liang, Chengzhu; Xu, Biao; Geng, Juan; Wang, Fengmei; Zhang, Xiaomei; Cheng, Gang

    2014-06-01

    A highly sensitive method using ultra-fast liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry (UFLC-Q/Trap MS) was developed to simultaneously screen and confirm nine beta-blockers (BBs) in porcine tissues (porcine muscle, liver and kidney). The method was used for trace determination of atenolol, pindolol, acebutolol, metoprolol, carazolol, labetalol, bisoprolol, propranolol and penbutolol. The homogenized tissues were hydrolyzed by beta-glucuronidase/aryl sulfatase and extracted with acetonitrile, followed by continuous purification procedures of disperse solid phase extraction (d-SPE) with diatomaceous earth and BondElut cartridge. The ultra-fast chromatographic separation was conducted on a Kinetex C18-XB column (150 mm x 2.1 mm, 2.6 microm) using 0.1% (v/v) formic acid aqueous solution and methanol as mobile phases in gradient elution. The optimized ion transitions were mployed in the mixed-mode of scheduled multiple reaction monitoring (sMRM) -information dependent acquisition (IDA)-enhanced product ion (EPI) scan. Qualification analysis was performed through spectra-matching with on-line lab-built MS/MS library. For quantification stable isotope-labelled analogues of the analytes were used as internal standards. As a result, in porcine liver, kidney and muscle, the nine BBs showed good linearity with all the correlation coefficients (r) more than 0.995 in the range of 0.1-20 microg/L. The limits of quantification (LOQ, S/N > or = 10) were 0.5 kg/kg for all the analytes. The developed method gave average recoveries of 87.5%-111.8% spiked at 0.5, 1.0 and 5.0 microg/kg with the relative standard deviations of 4.0%-12. 5%. The proposed method can be used to screen and confirm the nine BBs in a single run, which makes it effective in surveillance and detection of the BBs residues in porcine tissues. PMID:25269253

  10. Study of the in vitro metabolism of TJ0711 using ultra high performance liquid chromatography with quadrupole time-of-flight and ultra fast liquid chromatography with quadrupole linear ion trap mass spectrometry.

    PubMed

    Hu, Lei; Lv, Zhenhua; Li, Gao; Xu, Xiaolong; Zhang, Chenghao; Cao, Peng; Huang, Jiangeng; Si, Luqin

    2015-06-01

    TJ0711 (1-[4-(2-methoxyethyl)phenoxy]-3-[2-(2-methoxyphenoxy)ethylamino]-2-propanol) is a novel β-adrenoreceptor blocker with vasodilating activity. The aim of this study was to investigate the in vitro metabolic properties of TJ0711 from both qualitative and quantitative aspects using mouse, rat, dog, and human liver microsomes as well as rat hepatocytes. Two modern liquid chromatography with tandem mass spectrometry systems, ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry and ultra fast liquid chromatography with quadrupole linear ion trap mass spectrometry, were utilized for the analysis. To better characterize the metabolic pathways of TJ0711, two major metabolites were incubated under the same conditions as that for TJ0711. TJ0711 was extensively metabolized in vitro, and a total of 34 metabolites, including 19 phase I and 15 phase II metabolites, were identified. Similar metabolite profiles were observed among species, and demethylation, hydroxylation, carboxylic acid formation, and glucuronidation were proposed as the major metabolic routes. Significant interspecies differences were observed in the metabolic stability studies of TJ0711. Furthermore, gender differences were significant in mice, rats, and dogs, but were negligible in humans. The valuable information provided in this work will be useful in planning and interpreting further pharmacokinetic, in vivo metabolism and toxicological studies of this novel β-blocker. PMID:25800512

  11. Ion trap device

    DOEpatents

    Ibrahim, Yehia M.; Smith, Richard D.

    2016-01-26

    An ion trap device is disclosed. The device includes a series of electrodes that define an ion flow path. A radio frequency (RF) field is applied to the series of electrodes such that each electrode is phase shifted approximately 180 degrees from an adjacent electrode. A DC voltage is superimposed with the RF field to create a DC gradient to drive ions in the direction of the gradient. A second RF field or DC voltage is applied to selectively trap and release the ions from the device. Further, the device may be gridless and utilized at high pressure.

  12. Simultaneous determination of 18 preservative residues in vegetables by ultra high performance liquid chromatography coupled with triple quadrupole/linear ion trap mass spectrometry using a dispersive-SPE procedure.

    PubMed

    Zhou, Xue; Cao, Shurui; Li, Xianliang; Tang, Bobin; Ding, Xiaowen; Xi, Cunxian; Hu, Jiangtao; Chen, Zhiqiong

    2015-05-01

    A new method combining dispersive-solid phase purification procedure with ultra high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry was developed for simultaneous determination of 18 preservative residues in vegetables. The new method not only had the advantages of dispersive-solid phase purification procedure such as high recoveries, easy operation, rapid analysis, little solvent usage and wide analysis range of preservatives, but also had the advantages of ultra high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry to be operated in positive mode and negative mode simultaneously. The method was validated for the following representative matrices: radish (tuber), tomato (eggplant fruit), cabbage (leafy), cowpea (bean), cucumber (melon) and so on. Samples were extracted with hexane-ethyl acetate (1:2, v/v), and then detected by ultra high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry after being cleaned up with dispersive-solid phase purification procedure. Significant matrix effects were compensated by using the matrix-matched calibration curves. 18 preservatives showed good linearity over the range of 5.0-100.0 μg/L with correlation coefficients of 0.9904-1.000. The limits of detections were in the range of 0.04-4.16 μg/kg and the limits of quantity were in the range of 0.13-13.85 μg/kg. The recoveries of 18 preservatives ranged from 76.0% to 120.0% with the spiked levels of 2, 4 and 10 μg/kg into homogenized vegetables, and the relative standard deviations (RSDs) ranged from 0.3% to 14.8%. Compared with the reported literatures, the method is more rapid, simple, highly sensitive, reliable and can meet testing requirements of 18 preservative residues in vegetables. PMID:25797719

  13. Ultra high performance liquid chromatography with ion-trap TOF-MS for the fast characterization of flavonoids in Citrus bergamia juice.

    PubMed

    Sommella, Eduardo; Pepe, Giacomo; Pagano, Francesco; Tenore, Gian Carlo; Dugo, Paola; Manfra, Michele; Campiglia, Pietro

    2013-10-01

    We have developed a fast ultra HPLC with ion-trap TOF-MS method for the analysis of flavonoids in Citrus bergamia juice. With respect to the typical methods for the analysis of these matrices based on conventional HPLC techniques, a tenfold faster separation was attained. The use of a core-shell particle column ensured high resolution within the fast analysis time of only 5 min. Unambiguous determination of flavonoid identity was obtained by the employment of a hybrid ion-trap TOF mass spectrometer with high mass accuracy (average error 1.69 ppm). The system showed good retention time and peak area repeatability, with maximum RSD% values of 0.36 and 3.86, respectively, as well as good linearity (R(2) ≥ 0.99). Our results show that ultra HPLC can be a useful tool for ultra fast qualitative/quantitative analysis of flavonoid compounds in citrus fruit juices. PMID:23922323

  14. Peptide profiling of Internet-obtained Cerebrolysin using high performance liquid chromatography - electrospray ionization ion trap and ultra high performance liquid chromatography - ion mobility - quadrupole time of flight mass spectrometry.

    PubMed

    Gevaert, Bert; D'Hondt, Matthias; Bracke, Nathalie; Yao, Han; Wynendaele, Evelien; Vissers, Johannes Petrus Cornelis; De Cecco, Martin; Claereboudt, Jan; De Spiegeleer, Bart

    2015-09-01

    Cerebrolysin, a parenteral peptide preparation produced by controlled digestion of porcine brain proteins, is an approved nootropic medicine in some countries. However, it is also easily and globally available on the Internet. Nevertheless, until now, its exact chemical composition was unknown. Using high performance liquid chromatography (HPLC) coupled to ion trap and ultra high performance liquid chromatography (UHPLC) coupled to quadrupole-ion mobility-time-of-flight mass spectrometry (Q-IM-TOF MS), combined with UniProt pig protein database search and PEAKS de novo sequencing, we identified 638 unique peptides in an Internet-obtained Cerebrolysin sample. The main components in this sample originate from tubulin alpha- and beta-chain, actin, and myelin basic protein. No fragments of known neurotrophic factors like glial cell-derived neurotrophic factor (GDNF), neurotrophin nerve growth factor (NGF), brain-derived neurotrophic factor (BDNF), and ciliary neurotrophic factor (CNTF) were found, suggesting that the activities reported in the literature are likely the result of new, hitherto unknown cryptic peptides with nootropic properties. PMID:26017115

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

    PubMed

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

    2016-04-01

    In this paper, a wide scope screening method of pesticides in wine was established using liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QTOF MS) and liquid chromatography/quadrupole linear ion trap mass spectrometry (LC-QqLIT MS). Information dependent acquisition (IDA) experiments are used to obtain both MS and MS/MS information for LC-QTOF MS analysis. For LC-QqLIT MS analysis, MS/MS spectra of target pesticides were simultaneously acquired using Enhanced Product Ion (EPI) mode at very low concentrations to increase the confidence in analytical results of multiple reaction monitoring (MRM) by library searching. Method validation was carried out using 50 pesticides commonly used in vineyards. The LOQs, linearity, repeatability were determined and good enough for quantification. The screening and quantification results obtained using LC-QTOF MS and LC-QqLIT MS were compared. Contaminants were screened against libraries containing over 2800 compounds based on accurate mass, isotopic patterns, and MS/MS spectra searching to extend the scope of this methodology to non-target screening. PMID:26593613

  16. Nonlinear integrable ion traps

    SciTech Connect

    Nagaitsev, S.; Danilov, V.; /SNS Project, Oak Ridge

    2011-10-01

    Quadrupole ion traps can be transformed into nonlinear traps with integrable motion by adding special electrostatic potentials. This can be done with both stationary potentials (electrostatic plus a uniform magnetic field) and with time-dependent electric potentials. These potentials are chosen such that the single particle Hamilton-Jacobi equations of motion are separable in some coordinate systems. The electrostatic potentials have several free adjustable parameters allowing for a quadrupole trap to be transformed into, for example, a double-well or a toroidal-well system. The particle motion remains regular, non-chaotic, integrable in quadratures, and stable for a wide range of parameters. We present two examples of how to realize such a system in case of a time-independent (the Penning trap) as well as a time-dependent (the Paul trap) configuration.

  17. Separation and analysis of phenolic acids from Salvia miltiorrhiza and its related preparations by off-line two-dimensional hydrophilic interaction chromatography×reversed-phase liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    PubMed

    Sun, Wanyang; Tong, Ling; Miao, Jingzhuo; Huang, Jingyi; Li, Dongxiang; Li, Yunfei; Xiao, Hongting; Sun, Henry; Bi, Kaishun

    2016-01-29

    Salvia miltiorrhiza (SM) is one of the most widely used Traditional Chinese Medicine. Active constituents of SM mainly contain hydrophilic phenolic acids (PAs) and lipophilic tanshinones. However, due to the existing of multiple ester bonds and unsaturated bonds in the structures, PAs have numerous chemical conversion products. Many of them are so low-abundant that hard to be separated using conventional methods. In this study, an off-line two-dimensional liquid chromatography (2D-LC) method was developed to separate PAs in SM and its related preparations. In the first dimension, samples were fractionated by hydrophilic interaction chromatography (HILIC) (Acchrom×Amide, 4.6×250mm, 5μm) mainly based on the hydrogen bonding effects. The fractions were then separated on reversed-phase liquid chromatography (RP-LC) (Acquity HSS T3, 2.1×50mm, 1.7μm) according to hydrophobicity. For the selective identification of PAs, diode array detector (DAD) and electrospray ionization tandem ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) were employed. Practical and effective peak capacities of all the samples were greater than 2046 and 1130, respectively, with the orthogonalities ranged from 69.7% to 92.8%, which indicated the high efficiency and versatility of this method. By utilizing the data post-processing techniques, including mass defect filter, neutral loss filter and product ion filter, a total of 265 compounds comprising 196 potentially new PAs were tentatively characterized. Twelve kinds of derivatives, mainly including glycosylated compounds, O-alkylated compounds, condensed compounds and hydrolyzed compounds, constituted the novelty of the newly identified PAs. The HILIC×RP-LC/TOF-MS system expanded our understanding on PAs of S. miltiorrhiza and its related preparations, which could also benefit the separation and characterization of polar constituents in complicated herbal extracts. PMID:26792448

  18. Multi-mycotoxin Analysis of Finished Grain and Nut Products Using Ultrahigh-Performance Liquid Chromatography and Positive Electrospray Ionization-Quadrupole Orbital Ion Trap High-Resolution Mass Spectrometry.

    PubMed

    Liao, Chia-Ding; Wong, Jon W; Zhang, Kai; Yang, Paul; Wittenberg, James B; Trucksess, Mary W; Hayward, Douglas G; Lee, Nathaniel S; Chang, James S

    2015-09-23

    Ultrahigh-performance liquid chromatography using positive electrospray ionization and quadrupole orbital ion trap high-resolution mass spectrometry was evaluated for analyzing mycotoxins in finished cereal and nut products. Optimizing the orbital ion trap mass analyzer in full-scan mode using mycotoxin-fortified matrix extracts gave mass accuracies, δM, of < ± 2.0 ppm at 70,000 full width at half maximum (FWHM) mass resolution (RFWHM). The limits of quantitation were matrix- and mycotoxin-dependent, ranging from 0.02 to 11.6 μg/kg. Mean recoveries and standard deviations for mycotoxins from acetonitrile/water extraction at their relevant fortification levels were 91 ± 10, 94 ± 10, 98 ± 12, 91 ± 13, 99 ± 15, and 93 ± 17% for corn, rice, wheat, almond, peanut, and pistachio, respectively. Nineteen mycotoxins with concentrations ranging from 0.3 (aflatoxin B1 in peanut and almond) to 1175 μg/kg (fumonisin B1 in corn flour) were found in 35 of the 70 commercial grain and nut samples surveyed. Mycotoxins could be identified at δM < ± 5 ppm by identifying the precursor and product ions in full-scan MS and data-dependent MS/MS modes. This method demonstrates a new analytical approach for monitoring mycotoxins in finished grain and nut products. PMID:25531669

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

    PubMed

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

    2016-09-15

    A high-throughput method for simultaneous qualitative and quantitative analysis of 21 mycotoxins in Radix Paeoniae Alba (RPA) was developed by coupling the modified QuEChERS method with ultra-high performance liquid chromatography quadrupole linear ion trap mass spectrometry (UHPLC-QqLIT-MS). The 21 mycotoxins were extracted and cleaned up using QuEChERS-based procedure, then further separated on a C18 column and detected by a hybrid triple quadrupole linear ion trap mass spectrometer equipped with electrospray ionization source in the multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode. Under this technique, 13 mycotoxins were detected using acetonitrile and water containing 0.1% formic acid as the mobile phase in positive mode while the other 8 mycotoxins were detected using acetonitrile and water containing 0.1% ammonia as the mobile phase in negative mode. The calibration curves of all analytes showed good linearity (r(2)>0.995) within test ranges. The limits of detection and quantification ranged from 0.031 to 5.4μg/kg and 0.20 to 22μg/kg, respectively. Additionally, recoveries were all above 75.3% with relative standard deviations within 15%. The method proposed herein with significant advantages including simple pretreatment, rapid determination as well as high sensitivity, accuracy and throughput would be a preferred candidate for the determination and quantification of multi-class mycotoxin contaminants in real samples. PMID:27500642

  20. Direct quantitative analysis of organic compounds in the gas and particle phase using a modified atmospheric pressure chemical ionization source in combination with ion trap mass spectrometry.

    PubMed

    Warscheid, Bettina; Kückelmann, Ulrich; Hoffmann, Thorsten

    2003-03-15

    A slightly modified atmospheric pressure chemical ionization source is employed for direct quantitative analysis of volatile or semivolatile organic compounds in air. The method described here is based on the direct introduction of an analyte in the gas or particle phase, or both, into the ion source of a commercial ion trap mass spectrometer. For quantitation, a standard solution is directly transferred into the vaporizer unit of the ion source via a deactivated fused-silica capillary by using the sheath liquid syringe pump, which is part of the mass spectrometer. The standard addition procedure is conducted by varying the pump rate of a diluted solution of the standard compound in methanol/water. A N2 sheath gas flow is applied for optimal vaporization and mixing with the analyte gas stream. By performing detailed reagent ion monitoring experiments, it is shown that the relative signal intensity of [M + H]+ ions is dependent on the relative humidity of the analyte gas stream as well as the composition and concentration of CI reagent ions. The method is validated by a comparison of the standard addition results with a calibration test gas of known concentration. To demonstrate the potential of atmospheric pressure chemical ionization mass spectrometry as a quantitative analytical technique for on-line investigations, a tropospherically relevant reaction is carried out in a 493-L reaction chamber at atmospheric pressure and 296 K in synthetic air at 50% relative humidity. Finally, the applicability of the technique to rapidly differentiate between analytes in the gas and particle phase is demonstrated. PMID:12659203

  1. Characterization and quantitative analysis of phenylpropanoid amides in eggplant (Solanum melongena L.) by high performance liquid chromatography coupled with diode array detection and hybrid ion trap time-of-flight mass spectrometry.

    PubMed

    Sun, Jing; Song, Yue-Lin; Zhang, Jing; Huang, Zheng; Huo, Hui-Xia; Zheng, Jiao; Zhang, Qian; Zhao, Yun-Fang; Li, Jun; Tu, Peng-Fei

    2015-04-01

    Eggplant (Solanum melongena L.) is a famous edible and medicinal plant. Despite being widely cultivated and used, data on certain parts other than the fruit are limited. The present study focused on the qualitative and quantitative analysis of the chemical constituents, particularly phenylpropanoid amides (PAs), in eggplant. The mass fragmentation patterns of PAs were proposed using seven authentic compounds with the assistance of a hybrid ion trap time-of-flight mass spectrometer. Thirty-seven compounds (27 PAs and 10 others) were detected and plausibly assigned in the different parts of eggplant. Afterward, a reliable method based on liquid chromatography coupled with diode array detection was developed, validated, and applied for the simultaneous determination of seven PAs and three caffeoylquinic acids in 17 batches of eggplant roots with satisfactory accuracy, precision, and reproducibility, which could not only provide global chemical insight of eggplant but also offer a reliable tool for quality control. PMID:25796999

  2. Determination of the Alternaria mycotoxin tenuazonic acid in cereals by high-performance liquid chromatography-electrospray ionization ion-trap multistage mass spectrometry after derivatization with 2,4-dinitrophenylhydrazine.

    PubMed

    Siegel, David; Rasenko, Tatjana; Koch, Matthias; Nehls, Irene

    2009-05-22

    Tenuazonic acid (TA) is a major Alternaria mycotoxin. In the present work a novel approach for the detection of TA in cereals by liquid chromatography-ion-trap multistage mass spectrometry after derivatization with 2,4-dinitrophenylhydrazine is described. The product of the derivatization reaction and its major MS(2) fragments were characterised by Fourier transform-ion cyclotron resonance tandem mass spectrometry. Without preconcentration, the established method features a limit of detection of 10 microg/kg using 2g of sample in a rapid workup procedure. Accuracy, precision and linearity were evaluated in the working range of 50-5000 microg/kg. TA was detected in 13 and quantified in 3 out of 27 cereal samples obtained from a local supermarket, the average content being 49 microg/kg (highest incidence: 851+/-41 microg/kg). PMID:19361805

  3. Measuring Gas-Phase Basicities of Amino Acids Using an Ion Trap Mass Spectrometer: A Physical Chemistry Laboratory Experiment

    ERIC Educational Resources Information Center

    Sunderlin, Lee S.; Ryzhov, Victor; Keller, Lanea M. M.; Gaillard, Elizabeth R.

    2005-01-01

    An experiment is performed to measure the relative gas-phase basicities of a series of five amino acids to compare the results to literature values. The experiments use the kinetic method for deriving ion thermochemistry and allow students to perform accurate measurements of thermodynamics in a relatively short time.

  4. Multiplex gas chromatography

    NASA Technical Reports Server (NTRS)

    Valentin, Jose R.

    1990-01-01

    The principles of the multiplex gas chromatography (GC) technique, which is a possible candidate for chemical analysis of planetary atmospheres, are discussed. Particular attention is given to the chemical modulators developed by present investigators for multiplex GC, namely, the thermal-desorption, thermal-decomposition, and catalytic modulators, as well as to mechanical modulators. The basic technique of multiplex GC using chemical modulators and a mechanical modulator is demonstrated. It is shown that, with the chemical modulators, only one gas stream consisting of the carrier in combination with the components is being analyzed, resulting in a simplified instrument that requires relatively few consumables. The mechanical modulator demonstrated a direct application of multiplex GC for the analysis of gases in atmosphere of Titan at very low pressures.

  5. Determination of amphetamine-type stimulants, cocaine and ketamine in human hair by liquid chromatography/linear ion trap-Orbitrap hybrid mass spectrometry.

    PubMed

    Miyaguchi, Hajime; Inoue, Hiroyuki

    2011-09-01

    An LTQ Orbitrap XL hybrid mass spectrometry method was developed for the determination of illicit drugs and their metabolites, including amphetamine (AP), methamphetamine (MA), dimethylamphetamine (DMA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), ketamine (KET), norketamine (NK), cocaine (COC) and benzoylecgonine (BE), in hair. Micropulverized extraction was employed for sample preparation using a small hair sample (2 cm piece or 0.2 mg). Recoveries of the analytes during sample preparation were estimated using fortified hair samples and ranged from 35.5% for COC to 71.7% for AP. High resolution full-scan mass spectra and unit resolution product-ion spectra were obtained with the Orbitrap analyzer and the linear ion-trap analyzer, respectively. High-resolution extracted ion chromatograms at a tolerance of 3 ppm were utilized for quantification. The analytes were identified using the product-ion spectra in combination with the accurate masses of the corresponding protonated molecules observed in the high-resolution mass spectra. Lower limits of quantification obtained from a 0.2 mg hair sample were 0.050 ng mg(-1) (MDMA, KET and BE), 0.10 ng mg(-1) (AP, MA, DMA, NK and COC) and 0.50 ng mg(-1) (MDA). Two reference materials were analyzed for verification, and segmental analysis of single strands of hair specimens from actual cases was performed. PMID:21331390

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

    PubMed

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

    2011-07-29

    A multiresidue method was developed for the quantification and confirmation of 70 pesticides in paddy field water. After its filtration, water was injected directly in a liquid chromatograph coupled to a hybrid triple quadrupole-linear ion trap-mass spectrometer (QqLIT). The list of target analytes included organophosphates, phenylureas, sulfonylureas, carbamates, conazoles, imidazolinones and others compounds widely used in different countries where rice is cropped. Detection and quantification limits achieved were in the range from 0.4 to 80 ng L(-1) and from 2 to 150 ng L(-1), respectively. Correlation coefficients for the calibration curves in the range 0.1-50 μg L(-1) were higher than 0.99 except for diazinon (0.1-25 μg L(-1)). Only 9 pesticides presented more than 20% of signal suppression/enhancement, no matrix effect was observed in the studied conditions for the rest of the target pesticides. The method developed was used to investigate the occurrence of pesticides in 59 water samples collected in paddy fields located in Spain and Uruguay. The study shows the presence of bensulfuron methyl, tricyclazole, carbendazim, imidacloprid, tebuconazole and quinclorac in a concentration range from 0.08 to 7.20 μg L(-1). PMID:21397903

  7. Characterization and quantification of 10-hydroxycamptothecine in Camptotheca acuminate and its medicinal preparation by liquid chromatography-ion trap mass spectrometry.

    PubMed

    Chen, Qinhua; Pan, Guangmin; Xiong, Lin; He, Hongsheng; Yang, Hangdong

    2013-12-01

    A rapid and sensitive method for the identification and quantification of 10-hydroxycamptothecine (HCPT) in Camptotheca acuminata Decne is described. The HCPT standard solution was directly infused into the ion trap mass spectrometers (IT/MS) for collecting the MS(n) spectra. The electrospray ionization (ESI) mass spectral fragmentation pathway of HCPT was proposed and the ESI-MS(n) fragmentation behavior of HCPT was deduced in detail. The major fragment ions of HCPT were confirmed by MS(n) in both negative ion and positive ion mode. The possible main cleavage pathway of fragment ions was studied. Quantification of HCPT was assigned in negative-ion mode at a product ion at m/z 363 → 319 by LC-MS. The LC-MS method was validated for linearity, sensitivity, accuracy and precision, and then used to determine the content of the HCPT. Lastly, the LC-MS method was successfully applied to determine HCPT in real samples of Camptotheca acuminate Decne and its medicinal preparation in the first time. PMID:23813501

  8. Metabolism of nitazoxanide in rats, pigs, and chickens: Application of liquid chromatography coupled to hybrid linear ion trap/Orbitrap mass spectrometer.

    PubMed

    Huang, Xianhui; Guo, Chunna; Chen, Zhangliu; Liu, Yahong; He, Limin; Zeng, Zhenling; Yan, Chaoqun; Pan, Guangfang; Li, Shuaipeng

    2015-09-01

    Nitazoxanide (NTZ) is a nitrothiazole benzamide compound with a broad activity spectrum against parasites, Gram-positive and Gram-negative anaerobic bacteria, and viruses. In this study, hybrid linear ion trap/Orbitrap mass spectrometer providing a high mass resolution and accuracy was used to investigate the metabolism of NTZ in rats, pigs, and chickens. The results revealed that acetylation and glucuronidation were the main metabolic pathways in rats and pigs, whereas acetylation and sulfation were the major metabolic pathways in chickens, which indicated interspecies variations in drug metabolism and elimination. With the accurate mass data and the characteristic MS(n) product ions, we identified six metabolites in which tizoxanide and hydroxylated tizoxanide were phase I metabolites and tizoxanide glucuronide, tizoxanide glucose, tizoxanide sulfate and hydroxyl tizoxanide sulfate were phase II metabolites. Hydroxylated tizoxanide and tizoxanide glucose were identified for the first time. All the comprehensive data were provided to make out the metabolism of NTZ in rats, pigs and chickens more clearly. PMID:26231678

  9. Determination of tylosins A, B, C and D in bee larvae by liquid chromatography coupled to ion trap-tandem mass spectrometry.

    PubMed

    Bernal, J; Martín, Ma T; Toribio, L; Martín-Hernández, R; Higes, M; Bernal, J L; Nozal, M J

    2011-06-01

    A LC-MS/MS method has been developed to simultaneously quantify tylosins A, B, C and D in bee larvae, compounds currently used to treat one of the most lethal diseases affecting honey bees around the world, American Foulbrood (AFB). The influence of different aqueous media, temperature and light exposure on the stability of these four compounds was studied. The analytes were extracted from bee larvae with methanol and chromatographic separation was achieved on a Luna C(18) (150 × 4.6 mm i.d.) using a ternary gradient composed of a diluted formic acid, methanol and acetonitrile mobile phase. To facilitate sampling, bee larvae were initially dried at 60°C for 4h and afterwards, they were diluted to avoid problems of pressure. MSD-Ion Trap detection was employed with electrospray ionization (ESI). The calibration curves were linear over a wide range of concentrations and the method was validated as sensitive, precise and accurate within the limits of quantification (LOQ, 1.4-4.0 ng/g). The validated method was successfully employed to study bee larvae in field tests of bee hives treated with two formulations containing tylosin. In both cases it was evident that the minimal inhibitory concentration (MIC) had been reached. PMID:21498134

  10. The application of 2-D dual nanoscale liquid chromatography and triple quadrupole-linear ion trap system for the identification of proteins.

    PubMed

    Tschäppät, Viviane; Varesio, Emmanuel; Signor, Luca; Hopfgartner, Gérard

    2005-09-01

    2-D nanoscale LC combined with a triple quadrupole-linear ion trap mass spectrometer was applied to the analysis of a complex peptide mixture. A 2-D dual nanoscale LC-MS/MS system was compared to a conventional one. Peptides were separated with a strong cation exchange (SCX) microcolumn in the first dimension and two C18 nanocolumns were used as second dimension. MS experiments were performed using information-dependent data acquisition, where two precursor ions were selected from an enhanced MS (EMS) or an enhanced multicharged ion (EMC) as survey scan. The major benefit of EMC instead of EMS was a two-fold reduction of the data file and a 15% increase of characterized proteins. The advantage of the 2-D dual nanoscale LC-MS/MS system versus the conventional 2-D nanoscale LC-MS/MS system was reflected in the significant increase of peptides which were successfully identified within the same time frame. The first factor contributing to this increase was that the mass spectrometer was collecting twice the number of relevant MS/MS data. The second factor is the use of twice the number of SCX salt fractions in the first dimension, allowing a better sample fractionation, thereby reducing the number of peptides transferred to the second chromatographic dimension per salt fraction. PMID:16224964

  11. Multiclass, multiresidue method for the detection of antibiotic residues in distillers grains by liquid chromatography and ion trap tandem mass spectrometry.

    PubMed

    De Alwis, Hemakanthi; Heller, David N

    2010-04-30

    The increased production of ethanol in the US has resulted in large amounts of distillers grains (DG) which is an excellent feed supplement for livestock. However, the use of antimicrobials during ethanol fermentation has led to a growing concern over the possibility of their residues remaining in DG. To enable the detection of antimicrobial residues, a robust LC-MS/MS method was developed that included 13 antibiotics of diverse chemistries, ampicillin, penicillin G, tetracycline, oxytetracycline, chlortetracycline, bacitracin A, virginiamycin M1, chloramphenicol, erythromycin A, clarithromycin, tylosin A, monensin A and streptomycin. The residues were extracted with an aqueous solution of EDTA and trichloroacetic acid followed by methanol. The combined extract was subjected to a two-track cleanup and concentration on either hydrophilic polymeric or weak cation exchange solid phase extraction cartridges. The extracts are analyzed by LC/ion trap tandem mass spectrometry. The method was validated in dry DG matrix. Absolute recoveries of the analytes ranged from 50 to 100%. Accuracy ranged from 89 to 111% based on calibration by processed standards. The limits of detection and relative standard deviation are satisfactory to support future surveillance studies. The method was subsequently tested in three different end-products of DG: distillers dry grains, distillers wet grains and distillers grains solubles. PMID:20304405

  12. Halo ion trap mass spectrometer.

    PubMed

    Austin, Daniel E; Wang, Miao; Tolley, Samuel E; Maas, Jeffrey D; Hawkins, Aaron R; Rockwood, Alan L; Tolley, H Dennis; Lee, Edgar D; Lee, Milton L

    2007-04-01

    We describe a novel radio frequency ion trap mass analyzer based on toroidal trapping geometry and microfabrication technology. The device, called the halo ion trap, consists of two parallel ceramic plates, the facing surfaces of which are imprinted with sets of concentric ring electrodes. Radii of the imprinted rings range from 5 to 12 mm, and the spacing between the plates is 4 mm. Unlike conventional ion traps, in which hyperbolic metal electrodes establish equipotential boundary conditions, electric fields in the halo ion trap are established by applying different radio frequency potentials to each ring. The potential on each ring can be independently optimized to provide the best trapping field. The halo ion trap features an open structure, allowing easy access for in situ ionization. The toroidal geometry provides a large trapping and analyzing volume, increasing the number of ions that can be stored and reducing the effects of space-charge on mass analysis. Preliminary mass spectra show resolution (m/Deltam) of 60-75 when the trap is operated at 1.9 MHz and 500 Vp-p. PMID:17335180

  13. Gas Phase Absorption Spectroscopy of C+60 and C+70 in a Cryogenic Ion Trap: Comparison with Astronomical Measurements

    NASA Astrophysics Data System (ADS)

    Campbell, E. K.; Holz, M.; Maier, J. P.; Gerlich, D.; Walker, G. A. H.; Bohlender, D.

    2016-05-01

    Recent low-temperature laboratory measurements and astronomical observations have proved that the fullerene cation {{{C}}}60+ is responsible for four diffuse interstellar bands (DIBs). These absorptions correspond to the strongest bands of the lowest electronic transition. The gas phase spectrum below 10 {{K}} is reported here for the full wavelength range encompassed by the electronic transition. The absorption spectrum of {{{C}}}70+, with its origin band at 7959.2 {{\\mathringA }}, has been obtained under similar laboratory conditions. Observations made toward the reddened star {HD} 183143 were used in a specific search for the absorption of these fullerene cations in diffuse clouds. In the case of {{{C}}}60+, one further band in the astronomical spectrum at 9348.5 \\mathringA is identified, increasing the total number of assigned DIBs to five. Numerous other {{{C}}}60+ absorptions in the laboratory spectrum are found to lie below the astronomical detection limit. Special emphasis is placed on the laboratory determination of absolute absorption cross-sections. For {{{C}}}60+ this directly yields a column density, N({{{C}}}60+), of 2× {10}13 {{{cm}}}-2 in diffuse clouds, without the need to rely on theoretical oscillator strengths. The intensity of the {{{C}}}70+ electronic transition in the range 7000–8000 Å is spread over many features of similar strength. Absorption cross-section measurements indicate that even for a similar column density, the individual absorption bands of {{{C}}}70+ will be too weak to be detected in the astronomical spectra, which is confirmed giving an upper limit of 2 {{m\\mathringA }} to the equivalent width. Based on observations obtained at the Canada‑France‑Hawaii Telescope (CFHT) which is operated by the National Research Council of Canada, the Institut National des Sciences de l’Univers of the Centre National de la Recherche Scientifique of France, and the University of Hawaii.

  14. Ultrahigh-performance liquid chromatography-ion trap mass spectrometry characterization of the steroidal saponins of Dioscorea panthaica Prain et Burkill and its application for accelerating the isolation and structural elucidation of steroidal saponins.

    PubMed

    Wang, Weihao; Zhao, Ye; Jing, Wenguang; Zhang, Jun; Xiao, Hui; Zha, Qin; Liu, An

    2015-03-01

    Dioscorea panthaica is a traditional Chinese medicinal herb used in the treatment of various physiological conditions, including cardiovascular disease, gastropathy and hypertension. Steroidal saponins (SS) are the main active ingredients of this herb and have effects on myocardial ischemia and cancer. The phytochemical evaluation of SS is both time-consuming and laborious, and the isolation and structural determination steps can be especially demanding. For this reason, the development of new methods to accelerate the processes involved in the identification, isolation and structural elucidation of SS is highly desirable. In this study, a new ultrahigh performance liquid chromatography-ion trap mass spectrometry (UHPLC-IT/MS(n)) method has been developed for the identification of the SS in D. panthaica Prain et Burkill. Notably, the current method can distinguish between spirostanol and furostanol-type compounds based on the fragmentation patterns observed by electrospray ionization-ion trap mass spectrometry (ESI-IT/MS(n)) analysis. UHPLC-IT/MS(n) was used to conduct a detailed investigation of the number, structural class and order of the sugar moieties in the sugar chains of the SS present in D. panthaica. The established fragmentation features were used to analyze the compounds found in the 65% ethanol fraction of the water extracts of D. panthaica. Twenty-three SS were identified, including 11 potential new compounds and six groups of isomers. Two of these newly identified SS were selected as representative examples, and their chemical structures were confirmed by (1)H and (13)C NMR analyses. This newly developed UHPLC-IT/MS(n) method therefore allowed for the efficient identification, isolation and structural determination of the SS in D. panthaica. PMID:25575790

  15. Mini ion trap mass spectrometer

    DOEpatents

    Dietrich, D.D.; Keville, R.F.

    1995-09-19

    An ion trap is described which operates in the regime between research ion traps which can detect ions with a mass resolution of better than 1:10{sup 9} and commercial mass spectrometers requiring 10{sup 4} ions with resolutions of a few hundred. The power consumption is kept to a minimum by the use of permanent magnets and a novel electron gun design. By Fourier analyzing the ion cyclotron resonance signals induced in the trap electrodes, a complete mass spectra in a single combined structure can be detected. An attribute of the ion trap mass spectrometer is that overall system size is drastically reduced due to combining a unique electron source and mass analyzer/detector in a single device. This enables portable low power mass spectrometers for the detection of environmental pollutants or illicit substances, as well as sensors for on board diagnostics to monitor engine performance or for active feedback in any process involving exhausting waste products. 10 figs.

  16. Mini ion trap mass spectrometer

    DOEpatents

    Dietrich, Daniel D.; Keville, Robert F.

    1995-01-01

    An ion trap which operates in the regime between research ion traps which can detect ions with a mass resolution of better than 1:10.sup.9 and commercial mass spectrometers requiring 10.sup.4 ions with resolutions of a few hundred. The power consumption is kept to a minimum by the use of permanent magnets and a novel electron gun design. By Fourier analyzing the ion cyclotron resonance signals induced in the trap electrodes, a complete mass spectra in a single combined structure can be detected. An attribute of the ion trap mass spectrometer is that overall system size is drastically reduced due to combining a unique electron source and mass analyzer/detector in a single device. This enables portable low power mass spectrometers for the detection of environmental pollutants or illicit substances, as well as sensors for on board diagnostics to monitor engine performance or for active feedback in any process involving exhausting waste products.

  17. Quantification of Biogenic and Anthropogenic Hydrocarbons using a Commercial Gas Chromatograph - Ion Trap Mass Spectrometer at a Ground Site near Fort McKay, AB

    NASA Astrophysics Data System (ADS)

    Tokarek, T. W.; Osthoff, H. D.

    2014-12-01

    The extraction of fossil fuels from the Alberta oil sands has been the focus of considerable attention due to its association with sizeable emissions of a variety of atmospheric pollutants, the magnitude and impacts of which are currently poorly constrained by observations. In order to more reliably estimate the magnitude and impact of these emissions, an intensive air quality measurement campaign, called "Fort McMurray Oil Sands Strategic Investigation of Local Sources" (FOSSILS), was conducted in the summer of 2013 as part of the Alberta-Canada joint oil sands monitoring program (JOSM) to identify and quantify emissions and their transformations from the Alberta oil sands. The challenge is that the region is surrounded by boreal forest, which provides a substantial background of biogenic hydrocarbons during summer. In this presentation, measurements of volatile organic compounds (VOCs) at the AMS13 ground site near Fort McKay, Alberta, from Aug 17 to Sept 6, 2013 using a commercial Griffin 450 gas chromatograph equipped with ion trap mass spectrometric detection and Tenax preconcentration are described. The combination of retention information and electron impact mass spectral data allowed unambiguous identification and quantification of the major biogenic monoterpenes, e.g., α and β-pinene, limonene, camphene, and 3Δ-carene, and of many anthropogenically derived hydrocarbons. Mixing ratios of biogenic hydrocarbons varied with time of day, temperature, and solar radiation, with maxima typically occurring at night, rationalized by nocturnal mixing heights and low mixing ratios of the nocturnal oxidants ozone (O3) and the nitrate radical (NO3). In contrast, mixing ratios of anthropogenic VOCs, e.g., benzene, toluene, ethyl benzene, and o-, p-, and m-xylene (BTEX), strongly depended on meteorological conditions, i.e., local wind direction. During episodes with high BTEX abundance, many additional high molecular weight hydrocarbons were observed which were not

  18. Multi-allergen detection in food by micro high-performance liquid chromatography coupled to a dual cell linear ion trap mass spectrometry.

    PubMed

    Monaci, Linda; Pilolli, Rosa; De Angelis, Elisabetta; Godula, Michal; Visconti, Angelo

    2014-09-01

    There is a raising demand for sensitive and high throughput MS based methods for screening purposes especially tailored to the detection of allergen contaminants in different food commodities. A challenging issue is represented by complex food matrices where the antibody-based kits commercially available might encounter objective limitations consequently to epitope masking phenomena due to a multitude of interfering compounds arising from the matrix. The performance of a method duly optimized for the extraction and simultaneous detection of soy, egg and milk allergens in a cookie food matrix by microHPLC-ESI-MS/MS, is herein reported. Thanks to the innovative configuration and the versatility shown by the dual cell linear ion trap MS used, the most intense and reliable peptide markers were first identified by untargeted survey experiment, and subsequently employed to design an ad hoc multi-target SRM method, based on the most intense transitions recorded for each selected precursor peptide. A sample extraction and purification protocol was optimized also including an additional step based on sonication, which resulted in a considerable improvement in the detection of milk allergen peptides. Data Dependent™ Acquisition scheme allowed to fill out a tentative list of potential peptide markers, which were further filtered upon fulfilling specific requirements. A total of eleven peptides were monitored simultaneously for confirmation purposes of each allergenic contaminant and the two most sensitive peptide markers/protein were selected in order to retrieve quantitative information. Relevant LODs were found to range from 0.1μg/g for milk to 0.3μg/g for egg and 2μg/g for soy. PMID:25042441

  19. Accurate mass screening and identification of emerging contaminants in environmental samples by liquid chromatography-hybrid linear ion trap Orbitrap mass spectrometry.

    PubMed

    Hogenboom, A C; van Leerdam, J A; de Voogt, P

    2009-01-16

    The European Reach legislation will possibly drive producers to develop newly designed chemicals that will be less persistent, bioaccumulative or toxic. If this innovation leads to an increased use of more hydrophilic chemicals it may result in higher mobilities of chemicals in the aqueous environment. As a result, the drinking water companies may face stronger demands on removal processes as the hydrophilic compounds inherently are more difficult to remove. Monitoring efforts will also experience a shift in focus to more water-soluble compounds. Screening source waters on the presence of (emerging) contaminants is an essential step in the control of the water cycle from source to tap water. In this article, some of our experiences are presented with the hybrid linear ion trap (LTQ) FT Orbitrap mass spectrometer, in the area of chemical water analysis. A two-pronged strategy in mass spectrometric research was employed: (i) exploring effluent, surface, ground- and drinking-water samples searching for accurate masses corresponding to target compounds (and their product ions) known from, e.g. priority lists or the scientific literature and (ii) full-scan screening of water samples in search of 'unknown' or unexpected masses, followed by MS(n) experiments to elucidate the structure of the unknowns. Applications of both approaches to emerging water contaminants are presented and discussed. Results are presented for target analysis search for pharmaceuticals, benzotriazoles, illicit drugs and for the identification of unknown compounds in a groundwater sample and in a polar extract of a landfill soil sample (a toxicity identification evaluation bioassay sample). The applications of accurate mass screening and identification described in this article demonstrate that the LC-LTQ FT Orbitrap MS is well equipped to meet the challenges posed by newly emerging polar contaminants. PMID:18771771

  20. Cryogenic ion trapping systems with surface-electrode traps

    NASA Astrophysics Data System (ADS)

    Antohi, P. B.; Schuster, D.; Akselrod, G. M.; Labaziewicz, J.; Ge, Y.; Lin, Z.; Bakr, W. S.; Chuang, I. L.

    2009-01-01

    We present two simple cryogenic rf ion trap systems in which cryogenic temperatures and ultra high vacuum pressures can be reached in as little as 12 h. The ion traps are operated either in a liquid helium bath cryostat or in a low vibration closed cycle cryostat. The fast turn around time and availability of buffer gas cooling made the systems ideal for testing surface-electrode ion traps. The vibration amplitude of the closed cycled cryostat was found to be below 106 nm. We evaluated the systems by loading surface-electrode ion traps with S88r+ ions using laser ablation, which is compatible with the cryogenic environment. Using Doppler cooling we observed small ion crystals in which optically resolved ions have a trapped lifetime over 2500 min.

  1. Identification of metabolites of gardenin A in rats by combination of high-performance liquid chromatography with linear ion trap-Orbitrap mass spectrometer based on multiple data processing techniques.

    PubMed

    Zhang, Jiayu; Wang, Fang; Cai, Wei; Zhang, Qian; Liu, Ying; Li, Yun; Liu, Rongrong; Cao, Guangshang

    2015-03-01

    Gardenin A is one of the less abundant hydroxylated polymethoxyflavonoids (OH-PMFs) in nature, and has many potential significant health benefits. In the present study, an efficient strategy was established using high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometer to profile the in vivo metabolic fate of gardenin A in rat plasma and various tissues. First, an online LC-MS(n) data acquisition method was developed to trace all the probable metabolites. Second, a combination of offline data processing methods including extracted ion chromatography and multiple mass defect filters was employed to screen the common and uncommon metabolites from the background noise and endogenous components. Finally, structures of the metabolites were elucidated based on an accurate mass measurement, the diagnostic product ions of PMFs, and relevant drug biotransformation knowledge. Based on the proposed strategy, a total of 26 metabolites were observed and characterized. The results indicate that some biotransformations, such as methylation, demethoxylation, demethylation, glucuronide conjugation, sulfate conjugation and their composite reactions, have been discovered for OH-PMFs. Moreover, some diagnostic biotransformation pathways are summarized. Overall, this study gives us a first insight into the in vivo metabolism of gardenin A. The study also provides a practical strategy for rapidly screening and identifying metabolites, which can be widely applied for the other biotransformations. PMID:25041995

  2. Determination and fingerprint analysis of steroidal saponins in roots of Liriope muscari (Decne.) L. H. Bailey by ultra high performance liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    PubMed

    Li, Yong-Wei; Qi, Jin; Wen-Zhang; Zhou, Shui-Ping; Yan-Wu; Yu, Bo-Yang

    2014-07-01

    Liriope muscari (Decne.) L. H. Bailey is a well-known traditional Chinese medicine used for treating cough and insomnia. There are few reports on the quality evaluation of this herb partly because the major steroid saponins are not readily identified by UV detectors and are not easily isolated due to the existence of many similar isomers. In this study, a qualitative and quantitative method was developed to analyze the major components in L. muscari (Decne.) L. H. Bailey roots. Sixteen components were deduced and identified primarily by the information obtained from ultra high performance liquid chromatography with ion-trap time-of-flight mass spectrometry. The method demonstrated the desired specificity, linearity, stability, precision, and accuracy for simultaneous determination of 15 constituents (13 steroidal glycosides, 25(R)-ruscogenin, and pentylbenzoate) in 26 samples from different origins. The fingerprint was established, and the evaluation was achieved using similarity analysis and principal component analysis of 15 fingerprint peaks from 26 samples by ultra high performance liquid chromatography. The results from similarity analysis were consistent with those of principal component analysis. All results suggest that the established method could be applied effectively to the determination of multi-ingredients and fingerprint analysis of steroid saponins for quality assessment and control of L. muscari (Decne.) L. H. Bailey. PMID:24798297

  3. 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.

    PubMed

    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

    2016-01-01

    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. PMID:27171066

  4. Metabolic profile of naringenin in the stomach and colon using liquid chromatography/electrospray ionization linear ion trap quadrupole-Orbitrap-mass spectrometry (LC-ESI-LTQ-Orbitrap-MS) and LC-ESI-MS/MS.

    PubMed

    Orrego-Lagarón, Naiara; Vallverdú-Queralt, Anna; Martínez-Huélamo, Miriam; Lamuela-Raventos, Rosa M; Escribano-Ferrer, Elvira

    2016-02-20

    Several biological activities (antioxidant, anti-inflammatory, anticarcinogenic) are attributed to naringenin (NAR)-a predominant flavonoid of citrus fruit and tomato-despite its low bioavailability after ingestion. NAR undergoes extensive metabolism when crossing the gastrointestinal tract, resulting in enteric, hepatic and microbial metabolites, some of them with recognized beneficial effects on human health. This study sought to provide new insights into the metabolism of NAR in regions of the gastrointestinal tract where it has been less studied: the stomach and colon. With this purpose, liquid chromatography coupled with an electrospray ionization hybrid linear ion trap quadrupole Orbitrap mass spectrometry technique (LC-ESI-LTQ-Orbitrap-MS) was used for an accurate identification of NAR metabolites, and liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) on a triple quadrupole was used for their identification and quantification. The combination of both analytical techniques provided a broader metabolic profile of NAR. As far as we know, this is the first in-depth metabolic profiling study of NAR in the stomach of mice. Three of the metabolites determined using the LC-LTQ-Orbitrap could not be identified by LC-ESI-MS/MS in stomach perfusion samples: apigenin, 3-(4-hydroxyphenyl) propionic acid and phloroglucinol. The number of colonic metabolites determined using the LTQ-Orbitrap-MS was more than twice the number identified by LC-ESI-MS/MS. PMID:26698229

  5. Microfabricated ion trap mass spectrometry for characterization of organics and potential biomarkers

    NASA Astrophysics Data System (ADS)

    Austin, Daniel

    Mass spectrometry is a powerful analytical technique with a strong history in planetary exploration, and is the method of choice for detection and identification of organic and biological molecules. MS instrumentation can also be combined with techniques such as gas chromatography, liquid chromatography, or chiral separation, which are particularly important for analysis of complex mixtures or possible homochirality. Ion traps have several inherent advantages, including speed of analysis (important for GC-MS), MS/MS capabilities (important to identification of unknown compounds), excellent sensitivity, and ease of coupling with ambient ionization techniques that are under development for biomolecule detection. We report on progress in using microfabrication techniques to produce radiofrequency quadrupole ion traps that are much smaller, lighter, and lower power than existing instruments. We produce ion traps using an assembly of two ceramic plates, the facing surfaces of which are lithographically patterned with electrodes. This approach allows great flexibility in the trap geometry, and we have demonstrated working mass spectrometers with quadrupole, linear, and toroidal trapping fields. The approach also allows correction of higher-order terms in the electric field. With this system, mass resolution of up to 1300 has been demonstrated, which is adequate for identification of a wide range of potential biomarkers. Capabilities such as tandem analysis have also been demonstrated. Of particular interest is an ion trap that contains both quadrupole and toroidal trapping regions simultaneously and coaxially. Ions can be trapped as a large reservoir in the toroidal region and introduced in small batches to the quadrupole region for mass analysis. This capability is particularly valuable where the sample of interest is very small, such as microfossil with trace organics, and where the organic inventory is both complex and unknown. Development and results of this device

  6. IDENTIFICATION OF MICROCYSTIN TOXINS FROM A STRAIN OF MICROCYSTIS AERUGINOSA BY LIQUID CHROMATOGRAPHY INTRODUCTION INTO A HYBRID LINEAR ION TRAP-FOURIER TRANSFORM ION CYCLOTRON RESONANCE MASS SPECTROMETER

    EPA Science Inventory

    The cyclic heptapeptide microcystin toxins produced by a strain of Microcystis aeruginosa that has not been investigated previously were separated by liquid chromatography and identified by high-accuracy m/z measurements of their [M + H]+ ions and the fragment i...

  7. Hows and whys of ion trapping

    SciTech Connect

    Allison, J.; Stepnowski, R.M.

    1987-09-15

    Why trap ions. The localization of a single atomic particle in a vacuum is one of the most fundamental problems of physics and one of enduring interest. Working in the gas phase at low pressures, the chemist has the opportunity to study a variety of phenomena, if such species of interest can be contained for a period of time. Ion traps provide a unique chemical system available for a variety of experiments. The authors describe the bases of the technology, its strengths and limitations, and examples of its use.

  8. Ion trapping study in eRHIC

    SciTech Connect

    Hao, Y.

    2011-03-28

    The ion trapping effect is an important beam dynamics issue in energy recovery linac (ERL). The ionized residue gas molecules can accumulate at the vicinity of the electron beam path and deteriorate the quality of the electron beam. In this paper, we present calculation results to address this issue in eRHIC and find best beam pattern to eliminate this effect. eRHIC is the future electron ion collider(EIC), which collides 5GeV to 30GeV electron beam from a new electron accelerator with the ion beam from existing RHIC ring. The electron accelerator adopts a multi-pass ERL, which contains 6 passes with 2 linacs per pass. The electron impacted ionization effect needs attention to ensure the quality of the electron beam. The high energy electrons ionize the residue gas in beam pipe. These ions may accumulate and are 'trapped' near the axis of the pipe where the electron beam passes, due to the interaction with the electron beam. The concentration of the ion may produce noticeable space charge field that affects the electron beam and neutralize the electron beam in the linacs. In the paper, we start with cross section of the ionization process and calculate the accumulation time, which are followed by the modeling to determine the criteria of the ion trapping. The ion trapping effect is determined by the longitudinal configuration of the electron bunches. The effect can be reduced or mitigate by some proper electron beam patterns. We will present these patterns with a linearized model. We present the linearized calculation on the ion motion in the cavity of multi-pass ERL and determine the stability of the ion motion from the results. We conclude that the ionized molecules won't accumulated in eRHIC linacs except both 40m ends. Electro-static clearing electrodes should be installed in those regions to remove the ions from accumulation.

  9. Determination of sulfonamide antibiotics and metabolites in liver, muscle and kidney samples by pressurized liquid extraction or ultrasound-assisted extraction followed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry (HPLC-QqLIT-MS/MS).

    PubMed

    Hoff, Rodrigo Barcellos; Pizzolato, Tânia Mara; Peralba, Maria do Carmo Ruaro; Díaz-Cruz, M Silvia; Barceló, Damià

    2015-03-01

    Sulfonamides are widely used in human and veterinary medicine. The presence of sulfonamides residues in food is an issue of great concern. Throughout the present work, a method for the targeted analysis of 16 sulfonamides and metabolites residue in liver of several species has been developed and validated. Extraction and clean-up has been statistically optimized using central composite design experiments. Two extraction methods have been developed, validated and compared: i) pressurized liquid extraction, in which samples were defatted with hexane and subsequently extracted with acetonitrile and ii) ultrasound-assisted extraction with acetonitrile and further liquid-liquid extraction with hexane. Extracts have been analyzed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry. Validation procedure has been based on the Commission Decision 2002/657/EC and included the assessment of parameters such as decision limit (CCα), detection capability (CCβ), sensitivity, selectivity, accuracy and precision. Method׳s performance has been satisfactory, with CCα values within the range of 111.2-161.4 µg kg(-1), limits of detection of 10 µg kg(-1) and accuracy values around 100% for all compounds. PMID:25618734

  10. High-performance liquid chromatography with diode array detection coupled to electrospray time-of-flight and ion-trap tandem mass spectrometry to identify phenolic compounds from a lemon verbena extract.

    PubMed

    Quirantes-Piné, R; Funes, L; Micol, V; Segura-Carretero, A; Fernández-Gutiérrez, A

    2009-07-10

    High-performance liquid chromatography with diode array and electrospray ionization mass spectrometric detection was used to carry out the comprehensive characterization of a lemon verbena extract with demonstrated antioxidant and antiinflammatory activity. Two different MS techniques have been coupled to HPLC: on one hand, time-of-flight mass spectrometry, and on the other hand, tandem mass spectrometry on an ion-trap. The use of a small particle size C18 column (1.8 microm) provided a great resolution and made possible the separation of several isomers. The UV-visible spectrophotometry was used to delimit the class of phenolic compound and the accurate mass measurements on time-of-flight spectrometer enabled to identify the compounds present in the extract. Finally, the fragmentation pattern obtained in MS-MS experiments confirmed the proposed structures. This procedure was able to determine many well-known phenolic compounds present in lemon verbena such as verbascoside and its derivatives, diglucuronide derivatives of apigenin and luteolin, and eukovoside. Also gardoside, verbasoside, cistanoside F, theveside, campneoside I, chrysoeriol-7-diglucuronide, forsythoside A and acacetin-7-diglucuronide were found for the first time in lemon verbena. PMID:19500792

  11. Identification and determination of 34 water-soluble synthetic dyes in foodstuff by high performance liquid chromatography-diode array detection-ion trap time-of-flight tandem mass spectrometry.

    PubMed

    Li, Xiu Qin; Zhang, Qing He; Ma, Kang; Li, Hong Mei; Guo, Zhen

    2015-09-01

    An accurate method combining high performance liquid chromatography (HPLC) with diode array detection (DAD) and ion-trap time-of-flight mass spectrometry (IT-TOF/MS) was developed for simultaneous identification and quantification of 34 water-soluble synthetic dyes in foodstuff. Fragmentation patterns of synthetic dyes were proposed based on IT-TOF/MS. The molecular ion [M+H](+) was not observed in the conventional single-stage mass spectra for most of synthetic dyes. The single-stage mass spectra of synthetic dyes all afforded the diagnostic ions [(M-nNa+nH)+H](+) or [(M-nNa+nH)-H](-) in the positive or negative mode. Doubly charged ions were the characteristic ions of azo dyes. An HPLC-DAD method was developed to analyze 34 synthetic dyes in foodstuffs. The limits of detection (LOD) for the dyes were 0.01-0.05 μg/mL. The recoveries were between 76.1% and 105.0% with a RSD ranging from 1.4% to 6.4%. This method was successfully applied to analyzing the 34 water-soluble synthetic dyes in 21 commercial foods. PMID:25842343

  12. Simultaneous Qualitative and Quantitative Analysis of Multiple Chemical Constituents in YiQiFuMai Injection by Ultra-Fast Liquid Chromatography Coupled with Ion Trap Time-of-Flight Mass Spectrometry.

    PubMed

    Liu, Chunhua; Ju, Aichun; Zhou, Dazheng; Li, Dekun; Kou, Junping; Yu, Boyang; Qi, Jin

    2016-01-01

    YiQiFuMai injection (YQFM) is a modern lyophilized powder preparation derived from the traditional Chinese medicine Sheng-mai san (SMS) used for treating cardiovascular diseases, such as chronic heart failure. However, its chemical composition has not been fully elucidated, particularly for the preparation derived from Ophiopogon japonicus. This study aimed to establish a systematic and reliable method to quickly and simultaneously analyze the chemical constituents in YQFM by ultra-fast liquid chromatography coupled with ion trap time-of-flight mass spectrometry (UFLC-IT-TOF/MS). Sixty-five compounds in YQFM were tentatively identified by comparison with reference substances or literature data. Furthermore, twenty-one compounds, including three ophiopogonins, fifteen ginsenosides and three lignans were quantified by UFLC-IT-TOF/MS. Notably, this is the first determination of steroidal saponins from O. japonicus in YQFM. The relative standard deviations (RSDs) of intra- and inter-day precision, reproducibility and stability were <4.9% and all analytes showed good linearity (R² ≥ 0.9952) and acceptable recovery of 91.8%-104.2% (RSD ≤ 5.4%), indicating that the methods were reliable. These methods were successfully applied to quantitative analysis of ten batches of YQFM. The developed approach can provide useful and comprehensive information for quality control, further mechanistic studies in vivo and clinical application of YQFM. PMID:27213307

  13. [An ultra-high-pressure liquid chromatography/linear ion trap-Orbitrap mass spectrometry method coupled with a diagnostic fragment ions-searching-based strategy for rapid identification and characterization of chemical components in Polygonum cuspidatum].

    PubMed

    Pan, Zhiran; Liang, Hailong; Liang, Chabhufi; Xu, Wen

    2015-01-01

    A method for qualitative analysis of constituents in Polygonum cuspidatum by ultra-high-pressure liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap MS) has been established. The methanol extract of Polygonum cuspidatumrn was separated on a Waters UPLC C18 column using acetonitrile-water (containing formic acid) eluting system and detected by LTQ-Orbitrap hybrid mass spectrometer in negative mode. The targeted components were further fragmented in LTQ and high accuracy data were acquired by Orbitrap MS. The summarized fragmentation pathways of typical reference components and a diagnostic fragment ions-searching-based strategy were used for detection and identification of the main phenolic components in Polygonum cuspidatum. Other clues such as nitrogen rule, even electron rule, degree of unsaturation rule and isotopic peak data were included for the structural elucidation as well. The whole analytical procedure was within 10 min and more than 30 components were identified or tentatively identified. This method is helpful for further phytochemical research and quality control on Polygonum cuspidatum and related preparations. PMID:25958663

  14. Unequivocal Enantiomeric Identification and Analysis of 10 Chiral Pesticides in Fruit and Vegetables by QuEChERS Method Combined With Liquid Chromatography-Quadruple/Linear Ion Trap Mass Spectrometry Determination.

    PubMed

    He, Zeying; Peng, Yi; Wang, Lu; Luo, Ming; Liu, Xiaowei

    2015-12-01

    In this research, 10 chiral pesticides in fruits and vegetables were simultaneously determined using chiral liquid chromatography triple quadrupole-linear ion trap hybrid mass spectrometry (LC-QqLIT). The QuEChERS method was applied for sample preparation, and an enhanced product ion (EPI) scan was used to acquire tandem mass spectrometry (MS/MS) spectra for the library search. Parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative standard deviation (RSD), and matrix effects were evaluated in five representative matrices (strawberry, leek, cowpea, tomato, and eggplant). Good linearity with coefficient of determination (r(2) ) ≥0.997 was obtained for all 20 enantiomers in these five matrices over the range from 1.0 to 250 µg L(-1) . All the recoveries at 5 and 50 µg kg(-1) (n = 5) ranged between 70% and 120% with RSD below 20%, indicating satisfactory precision. The LOQ for the enantiomers ranged between 0.05 and 1 µg kg(-1) . Based on the proposed method, 135 commonly consumed fruits and vegetables taken from markets in Guizhou province, China, were analyzed. Enantioselective degradation for the selected chiral pesticides was observed in most of the positive samples. PMID:26392120

  15. Qualitative and Quantitative Assessments of Aconiti Lateralis Radix Praeparata Using High-Performance Liquid Chromatography Coupled with Diode Array Detection and Hybrid Ion Trap-Time-of-Flight Mass Spectrometry.

    PubMed

    Zhang, Na; Song, Yuelin; Song, Qingqing; Shi, Shepo; Zhang, Qian; Zhao, Yunfang; Li, Jun; Tu, Pengfei

    2016-07-01

    Dual roles have been widely disclosed for Aconiti Lateralis Radix Praeparata (Chinese name: Fuzi) by acting as an effective herbal medicine accompanied with high toxicity risk and narrow therapeutic range. Aconite alkaloids, also known as diterpenoid alkaloids (DAs), have been proved to be primary therapeutic as well as toxic material basis of Fuzi. In the present study, we aim to characterize qualitative profile along with quantitative features of DAs in Fuzi, which could benefit the quality control of Fuzi as well as its safe medication in clinic. Chromatographic fingerprinting was achieved using 12 batches of crude materials collected from different habitats (similarities >0.9) by hyphenating liquid chromatography (LC) with diode array detection. Simultaneous determination of six primary DAs, namely benzoylmesaconine, benzoylaconine, benzoylhypaconine, mesaconine, aconitine and hypaconitine, was also carried out. The developed method was systematically validated and successfully applied for quantitative characterization. Significant variations were observed regarding the contents of those six analytes among different raw materials. A total of 99 DAs were detected and characterized, including 9 unambiguous identities and 77 putative assignments, as well as 13 unknown compounds, from the representative extract by LC coupled with hybrid ion trap-time-of-flight mass spectrometry. The findings obtained herein could favor in-depth understanding of the chemical composition of DAs and the quality control of Fuzi. PMID:27048641

  16. Chemometrics for comprehensive analysis of nucleobases, nucleosides, and nucleotides in Siraitiae Fructus by hydrophilic interaction ultra high performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry.

    PubMed

    Zhou, Guisheng; Wang, Mengyue; Xu, Renjie; Li, Xiao-Bo

    2015-10-01

    A rapid and sensitive hydrophilic interaction ultra high performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry method was validated for the simultaneous determination of 20 nucleobases, nucleosides, and nucleotides (within 3.5 min), and then was employed to test the functional food of Luo-Han-Guo samples. The analysis showed that the Luo-Han-Guo was rich in guanosine and uridine, but contained trace levels of the other target compounds. Chemometrics methods were employed to identify 40 batches of Luo-Han-Guo samples from different cultivated forms, regions and varieties. Unsupervised hierarchical cluster analysis and principal component analysis were used to classify Luo-Han-Guo samples based on the level of the 20 target compounds, and the supervised learning method of counter propagation artificial neural network was utilized to further separate clusters and validate the established model. As a result, the samples could be clustered into three primary groups, in which correlation with cultivated varieties was observed. The present strategy could be applied to the investigation of other edible plants containing nucleobases, nucleosides, or nucleotides. PMID:26249158

  17. Comprehensive characterization of the in vitro and in vivo metabolites of geniposide in rats using ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometer.

    PubMed

    Li, Yun; Cai, Wei; Cai, Qian; Che, Yanyun; Zhao, Baosheng; Zhang, Jiayu

    2016-01-01

    1. Geniposide (genipin 1-O-glucose), one of the major bioactive constituents isolated from Fructus Gardeniae, possesses many biological activities. In this study, an efficient strategy was developed using ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometer (UPLC-LTQ-Orbitrap) to profile the in vitro and in vivo metabolic patterns of geniposide in rat liver microsomes (RLMs), plasma, urine, and various tissues. And post-acquisition data-mining methods including extracted ion chromatogram (EIC), multiple mass defect filters (MMDF), fragment ion searching (FISh), and isotope pattern filtering (IPF) were adopted to characterize the known and unknown metabolites. 2. A total of 33 metabolites were detected and interpreted according to accurate mass measurement, diagnostic fragment ions, relevant drug biotransformation knowledge, and bibliography data. Among them, 17 metabolites were detected in the plasma, 31 metabolites were identified in the urine, six metabolites could be found in rat heart, 12 in liver, three in spleen, six in lung, 12 in kidney, six in brain, and four in RLMs. 3. A series of corresponding reactions such as hydrolysis, hydroxylation, taurine conjugation, hydrogenation, decarboxylation, demethylation, sulfate conjugation, cysteine S-conjugation, glucosylation, and their composite reactions were all discovered. 4. The results could provide comprehensive insights and guidance for elucidation of side effect mechanism and safety monitoring as well as for rational formulation design in drug delivery system. The newly discovered geniposide metabolites could be targets for future metabolism studies on the important chemical constituents from herbal medicines. PMID:26330181

  18. Metabolism studies of the Kratom alkaloids mitraciliatine and isopaynantheine, diastereomers of the main alkaloids mitragynine and paynantheine, in rat and human urine using liquid chromatography-linear ion trap-mass spectrometry.

    PubMed

    Philipp, Anika A; Wissenbach, Dirk K; Weber, Armin A; Zapp, Josef; Maurer, Hans H

    2011-05-01

    Mitragyna speciosa (Kratom in Thai), native in Southeast Asia, is increasingly misused as a herbal drug of abuse. During metabolism studies on the Kratom alkaloids mitragynine, its diastereomers speciogynine and speciociliatine as well as paynantheine in rats and humans, further isomeric compounds were detected in Kratom users' urine. The question arose whether these compounds were formed from the low abundant, isomeric alkaloids mitraciliatine (MC) and isopaynantheine (ISO-PAY). Therefore, the aim of the presented study was to identify using liquid chromatography-linear ion trap-mass spectrometry their phase I and II metabolites in rat urine after administration of pure MC or ISO-PAY, to confirm their formation in humans, and finally to confirm whether the above-mentioned isomeric compounds in human urine represent MC and ISO-PAY and/or their metabolites. The metabolic pathways of both alkaloids in rats were found to be comparable to those of their corresponding diastereomers. In the human urines tested, not all metabolites found in rats could be detected because of the much lower amounts of MC and ISO-PAY in Kratom. However, all the above-mentioned so far unknown isomeric compounds could be identified in the human urine samples as MC, ISO-PAY and/or their metabolites. The used LC separation was also suitable for the differentiation of all other Kratom alkaloids and their metabolites in human urine. PMID:21450536

  19. Dispersive liquid-liquid microextraction for the determination of macrocyclic lactones in milk by liquid chromatography with diode array detection and atmospheric pressure chemical ionization ion-trap tandem mass spectrometry.

    PubMed

    Campillo, Natalia; Viñas, Pilar; Férez-Melgarejo, Gema; Hernández-Córdoba, Manuel

    2013-03-22

    Eprinomectin (EPRI), abamectin (ABA), doramectin (DOR), moxidectin (MOX) and ivermectin (IVM) were determined in milk samples using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography with diode array detection (LC-DAD) coupled to atmospheric pressure chemical ionization in negative ion mode ion-trap tandem mass spectrometry (APCI-IT-MS/MS). Milk proteins were removed by precipitation with trichloroacetic acid and the analytes were preconcentrated using 2mL of acetonitrile containing 200μL of chloroform as extraction mixture. The effect of several parameters for the liquid-liquid microextraction efficiency was evaluated. Standard additions method was used for quantification purposes, the correlation coefficients were better than 0.9970 in all cases and the quantification limits ranged from 1.0 to 4.7ngg(-1) and from 0.1 to 2.4ngg(-1) when using DAD and MS, respectively. The DLLME-LC-APCI-IT-MS/MS optimized method was successfully applied to different milk samples and none of the studied analytes was detected in the samples studied. The recoveries for milk samples spiked at concentration levels ranging between 0.5 and 50ngg(-1), depending on the compound, were between 89.5 and 105%, with relative standard deviations lower than 9% (n=135). Simplicity, rapidity and reliability are important advantages of the proposed method, while the sample preparation step can be regarded as environmentally friendly. PMID:23415139

  20. Microscale ion trap mass spectrometer

    DOEpatents

    Ramsey, J. Michael; Witten, William B.; Kornienko, Oleg

    2002-01-01

    An ion trap for mass spectrometric chemical analysis of ions is delineated. The ion trap includes a central electrode having an aperture; a pair of insulators, each having an aperture; a pair of end cap electrodes, each having an aperture; a first electronic signal source coupled to the central electrode; a second electronic signal source coupled to the end cap electrodes. The central electrode, insulators, and end cap electrodes are united in a sandwich construction where their respective apertures are coaxially aligned and symmetric about an axis to form a partially enclosed cavity having an effective radius r.sub.0 and an effective length 2z.sub.0, wherein r.sub.0 and/or z.sub.0 are less than 1.0 mm, and a ratio z.sub.0 /r.sub.0 is greater than 0.83.

  1. Improved sensitivity of ochratoxin A analysis in coffee using high-performance liquid chromatography with hybrid triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS).

    PubMed

    Kokina, Aija; Pugajeva, Iveta; Bartkevics, Vadims

    2016-04-01

    A novel and sensitive method utilising high-performance liquid chromatography coupled to triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS) was developed in order to analyse the content of ochratoxin A (OTA) in coffee samples. The introduction of the triple-stage MS scanning mode (MS(3)) has been shown to increase greatly sensitivity and selectivity by eliminating the high chromatographic baseline caused by interference of complex coffee matrices. The analysis included the sample preparation procedure involving extraction of OTA using a methanol-water mixture and clean-up by immunoaffinity columns and detection using the MS(3) scanning mode of LC-QqQLIT-MS/MS. The proposed method offered a good linear correlation (r(2) > 0.998), excellent precision (RSD < 2.9%) and recovery (94%). The limit of quantification (LOQ) for coffee beans and espresso beverages was 0.010 and 0.003 µg kg(-1), respectively. The developed procedure was compared with traditional methods employing liquid chromatography coupled to fluorescent and tandem quadrupole detectors in conjunction with QuEChERS and solid-phase extraction. The proposed method was successfully applied to the determination of OTA in 15 samples of coffee beans and in 15 samples of espresso coffee beverages obtained from the Latvian market. OTA was found in 10 samples of coffee beans and in two samples of espresso in the ranges of 0.018-1.80 µg kg(-1) and 0.020-0.440 µg l(-1), respectively. No samples exceeded the maximum permitted level of OTA in the European Union (5.0 µg kg(-1)). PMID:26933771

  2. Development and Evaluation of a Variable-Temperature Quadrupole Ion Trap Mass Spectrometer

    NASA Astrophysics Data System (ADS)

    Derkits, David; Wiseman, Alex; Snead, Russell F.; Dows, Martina; Harge, Jasmine; Lamp, Jared A.; Gronert, Scott

    2016-02-01

    A new, variable-temperature mass spectrometer system is described. By applying polyimide heating tape to the end-cap electrodes of a Bruker (Bremen, Germany) Esquire ion trap, it is possible to vary the effective temperature of the system between 40 and 100°C. The modification does not impact the operation of the ion trap and the heater can be used for extended periods without degradation of the system. The accuracy of the ion trap temperatures was assessed by examining two gas-phase equilibrium processes with known thermochemistry. In each case, the variable-temperature ion trap provided data that were in good accord with literature data, indicating the effective temperature in the ion trap environment was being successfully modulated by the changes in the set-point temperatures on the end-cap electrodes. The new design offers a convenient and effective way to convert commercial ion trap mass spectrometers into variable-temperature instruments.

  3. Development and Evaluation of a Variable-Temperature Quadrupole Ion Trap Mass Spectrometer.

    PubMed

    Derkits, David; Wiseman, Alex; Snead, Russell F; Dows, Martina; Harge, Jasmine; Lamp, Jared A; Gronert, Scott

    2016-02-01

    A new, variable-temperature mass spectrometer system is described. By applying polyimide heating tape to the end-cap electrodes of a Bruker (Bremen, Germany) Esquire ion trap, it is possible to vary the effective temperature of the system between 40 and 100°C. The modification does not impact the operation of the ion trap and the heater can be used for extended periods without degradation of the system. The accuracy of the ion trap temperatures was assessed by examining two gas-phase equilibrium processes with known thermochemistry. In each case, the variable-temperature ion trap provided data that were in good accord with literature data, indicating the effective temperature in the ion trap environment was being successfully modulated by the changes in the set-point temperatures on the end-cap electrodes. The new design offers a convenient and effective way to convert commercial ion trap mass spectrometers into variable-temperature instruments. PMID:26483183

  4. Localization of double bonds in triacylglycerols using high-performance liquid chromatography/atmospheric pressure chemical ionization ion-trap mass spectrometry.

    PubMed

    Háková, Eva; Vrkoslav, Vladimír; Míková, Radka; Schwarzová-Pecková, Karolina; Bosáková, Zuzana; Cvačka, Josef

    2015-07-01

    A method for localizing double bonds in triacylglycerols using high-performance liquid chromatography-tandem mass spectrometry with atmospheric pressure chemical ionization (APCI) was developed. The technique was based on collision-induced dissociation or pulsed Q collision-induced dissociation of the C3H5N(+•) adducts ([M + 55](+•)) formed in the presence of acetonitrile in the APCI source. The spectra were investigated using a large series of standards obtained from commercial sources and prepared by randomization. The fragmentation spectra made it possible to determine (i) the total number of carbons and double bonds in the molecule, (ii) the number of carbons and double bonds in acyls, (iii) the acyl in the sn-2 position on the glycerol backbone, and (iv) the double-bond positions in acyls. The double-bond positions were determined based on two types of fragments (alpha and omega ions) formed by cleavages of C-C bonds vinylic to the original double bond. The composition of the acyls and their positions on glycerol were established from the masses and intensities of the ions formed by the elimination of fatty acids from the [M + 55](+•) precursor. The method was applied for the analysis of triacylglycerols in olive oil and vernix caseosa. PMID:25701424

  5. Ion-pairing liquid chromatography with on-line electrospray ion trap mass spectrometry for the structural analysis of N-unsubstituted heparin/heparan sulfate.

    PubMed

    Du, Jia Yan; Chen, Lan Rong; Liu, Su; Lin, Jiang Hui; Liang, Qun Tao; Lyon, Malcolm; Wei, Zheng

    2016-08-15

    The rare N-unsubstituted glucosamine (GlcNH3(+)) residues in heparan sulfate (HS) have important biological and pathophysiological roles. In this study, a high-resolution method for the separation and analysis of N-unsubstituted disaccharides of heparin/HS is described. Four N-unsubstituted disaccharides, together with eight N-substituted species, can be well-separated by ion-pair reverse-phase ultra-performance liquid chromatography. Each disaccharide can then be detected and its relative abundance quantified using electrospray ionization mass spectrometry in the negative mode. Because of its high sensitivity, without interference from proteins and other sample impurities, this method is particularly useful in the analysis of low content GlcNH3(+) residues in small amounts of biological materials, eg. sera, tissue and cell culture-derived samples. This would lead to a better understanding of the biological origin of GlcNH3(+) residues and their increasingly important function in human health and disease. PMID:27322632

  6. Biotransformation and metabolic profile of buddleoside with human intestinal microflora by ultrahigh-performance liquid chromatography coupled to hybrid linear ion trap/orbitrap mass spectrometer.

    PubMed

    Tao, Jin-Hua; Duan, Jin-Ao; Jiang, Shu; Qian, Yi-Yun; Qian, Da-Wei

    2016-07-01

    Buddleoside (also known as linarin) as the major flavonoid in Chrysanthemum morifolium Ramat., has been reported to possess a wide range of pharmacological activities. The human intestinal microbiota might have an important impact on drug metabolism and ultimately on the drug oral bioavailability. However, the interaction of the buddleoside with human intestinal bacteria remains unknown. In this study, the conversion of buddleoside by different bacteria from human feces was firstly investigated. A reliable, sensitive and rapid analytical method, ultra performance liquid chromatography was established and successfully applied to investigate the metabolites and metabolic profile of buddleoside by human intestinal bacteria. Among the isolated bacteria, four strains including Escherichia sp. 4, Escherichia sp. 34, Enterococcus sp. 45 and Bacillus sp. 46 showed more powerful conversion capability. Based on the accurate mass data and the characteristic MS(n) product ions, the parent and six metabolites were detected and tentatively identified compared with blank samples. The metabolites were produced by four main metabolic pathways including deglycosylation, acetylation, methylation and hydroxylation. Buddleoside could be firstly converted to its aglycon acacetin (M2) by the majority of the isolated intestinal bacteria. Subsequently, M2 was further metabolize to its methylated (M3), acetylated (M4), hydroxylated (M5) and hydrogenated product (M6). However, acacetin-7-glucosid (M1) was obtained only from the minor bacterial samples like Bacillus sp. 46. To further explain the metabolism of buddleoside, the β-d-glucosidase and α-l-rhamnosidase activities of four strains were analyzed. Bacillus sp. 46 could only produce α-l-rhamnosidase, while the other three strains showed two kinds of enzyme activities. Furthermore, the activities of α-l-rhamnosidase and β-d-glucosidase reached the highest level at 12-18h and 10-12h, respectively. The metabolic routes and metabolites

  7. Simultaneous determination of 19 triazine pesticides and degradation products in processed cereal samples from Chinese total diet study by isotope dilution-high performance liquid chromatography-linear ion trap mass spectrometry.

    PubMed

    Li, Peng; Yang, Xin; Miao, Hong; Zhao, Yunfeng; Liu, Wei; Wu, Yongning

    2013-06-01

    A selective and sensitive isotope dilution-high performance liquid chromatography-linear ion trap mass spectrometry (Isotope Dilution-HPLC-LIT-MS(3)) method was developed for the simultaneous determination of 19 triazine pesticides and their degradation products in processed cereal samples from Chinese total diet study (TDS). The method integrated the addition of isotope internal standards, liquid-liquid extraction (LLE), clean-up with MCX solid-phase extraction (SPE) cartridges and HPLC-LIT-MS(3) analysis with selected reaction monitoring (SRM) mode. Matrix-matched calibration curves showed good linearity (R(2)≥0.9940) verified by applying the Mandel's fitting test (p>0.087) performed at the 95% confidence level. Decision limits (CCαs) and detection capabilities (CCβs) of the 19 triazine pesticides and their degradation products fell in the ranges of 0.0020-0.4200 μg kg(-1) and 0.0024-0.4500 μg kg(-1), respectively. Recoveries ranged from 70.1% to 112.8%, with the relative standard deviations (RSDs) ranging from 1.5% to 13.5%. Furthermore, the proposed method was applied to analyzing the proposed cereal samples from the fourth Chinese TDS. Eleven triazines were detected in six cereal samples with the concentrations ranging from 0.013 to 0.987 μg kg(-1). This method can also be used for the further determination of the triazines in other food group composites, and ultimately served as a methodological foundation for assessing the triazines in the average Chinese diet in the general population. PMID:23684466

  8. Use of liquid chromatography coupled to low- and high-resolution linear ion trap mass spectrometry for studying the metabolism of paynantheine, an alkaloid of the herbal drug Kratom in rat and human urine.

    PubMed

    Philipp, Anika A; Wissenbach, Dirk K; Weber, Armin A; Zapp, Josef; Zoerntlein, Siegfried W; Kanogsunthornrat, Jidapha; Maurer, Hans H

    2010-04-01

    The Thai medicinal plant Mitragyna speciosa (Kratom in Thai) is misused as a herbal drug of abuse. During studies on the main Kratom alkaloid mitragynine (MG) in rats and humans, several dehydro analogs could be detected in urine of Kratom users, which were not found in rat urine after administration of pure MG. Questions arose as to whether these compounds are formed from MG only by humans or whether they are metabolites formed from the second abundant Kratom alkaloid paynantheine (PAY), the dehydro analog of MG. Therefore, the aim of the presented study was to identify the phase I and II metabolites of PAY in rat urine after administration of the pure alkaloid. This was first isolated from Kratom leaves. Liquid chromatography-linear ion trap mass spectrometry provided detailed structure information of the metabolites in the MS(n) mode particularly with high resolution. Besides PAY, the following phase I metabolites could be identified: 9-O-demethyl PAY, 16-carboxy PAY, 9-O-demethyl-16-carboxy PAY, 17-O-demethyl PAY, 17-O-demethyl-16,17-dihydro PAY, 9,17-O-bisdemethyl PAY, 9,17-O-bisdemethyl-16,17-dihydro PAY, 17-carboxy-16,17-dihydro PAY, and 9-O-demethyl-17-carboxy-16,17-dihydro PAY. These metabolites indicated that PAY was metabolized via the same pathways as MG. Several metabolites were excreted as glucuronides or sulfates. The metabolism studies in rats showed that PAY and its metabolites corresponded to the MG-related dehydro compounds detected in urine of the Kratom users. In conclusion, PAY and its metabolites may be further markers for a Kratom abuse in addition of MG and its metabolites. PMID:19902190

  9. Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

    PubMed

    Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

    2016-08-12

    A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. PMID:27412322

  10. Characterization and quantification of monoterpenoids in different types of peony root and the related Paeonia species by liquid chromatography coupled with ion trap and time-of-flight mass spectrometry.

    PubMed

    Shi, Yan-Hong; Zhu, Shu; Ge, Yue-Wei; Toume, Kazufumi; Wang, Zhengtao; Batkhuu, Javzan; Komatsu, Katsuko

    2016-09-10

    Monoterpenoids with "cage-like" pinane skeleton are the unique and main bioactive constituents in peony root, the root of Paeonia lactiflora. A liquid chromatography coupled with ion trap and time-of-flight mass spectrometry (LC-IT-TOF-MS) method was developed for characterization and quantification of monoterpenoids in different types of peony root and the roots of related Paeonia species. MS/MS fragmentation patterns of monoterpenoids with paeoniflorin-, albiflorin- and sulfonated paeoniflorin-type of skeletons were elucidated, which provided basic clues enabling subsequent identification of 35 monoterpenoids in LC-MS profiles of Paeonia species. The profiling analysis and further quantification of 15 main monoterpenoids in 56 samples belonged to red peony root (RPR), white peony root (WPR), peony root in Japanese market (PR) and the roots of related Paeonia species revealed that paeoniflorin, benzoylpaeoniflorin, galloylpaeoniflorin, oxypaoniflorin and albiflorin were predominant constituents in all the samples; mudanpioside C was the characteristic component of P. lactiflora, and 4-O-methyl-paeoniflorin was only detected in P. veitchii and P. anomala. Total contents of the 15 monoterpenoids were obviously higher in the roots of P. lactiflora and P. veitchii than in those of P. anomala and P. japonica. Principal component analysis based on the quantitative results showed that the samples derived from P. lactiflora were clearly classified into RPR, WPR/PR, and sulfur-fumigated WPR groups, besides the respective group of P. veitchii and P. anomala. This study clarified the chemical characteristics of the respective type of peony root and the related Paeonia species, as well as the marker constituents for their discrimination. PMID:27521818

  11. Comparison of two ionic liquid dispersive liquid-liquid microextraction approaches for the determination of benzoylurea insecticides in wastewater using liquid chromatography-quadrupole-linear ion trap-mass spectrometry: evaluation of green parameters.

    PubMed

    Vázquez, M M Parrilla; Vázquez, P Parrilla; Galera, M Martínez; Moreno, A Uclés

    2014-08-22

    Two dispersive liquid-liquid microextraction (DLLME) approaches including temperature-controlled ionic liquid dispersive liquid-liquid microextraction (TCIL-DLLME) and ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (US-IL-DLLME) were compared for the extraction of six benzoylurea insecticides (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, lufenuron and flufenoxuron) from wastewater samples prior to their determination by high-performance liquid chromatography with a hybrid triple quadrupole-linear ion trap-mass spectrometer (LC-QqLIT-MS/MS). Influential parameters affecting extraction efficiency were systematically studied and optimized and the most significant green parameters were quantified and compared. The best results were obtained using the US-IL-DLLME procedure, which employed the IL 1-octyl-3-methylimidazolium hexafluorophosphate ([C8MIM][PF6]) and methanol (MeOH) as extraction and disperser solvent, respectively. US-IL-DLLME procedure was fast, easy, low environmental toxicity and, it was also able to successfully extract all selected benzoylureas. This method was extensively validated with satisfactory results: limits of detection and quantification were in the range 0.5-1.0 ng L(-1) and 1.5-3.5 ng L(-1), respectively, whereas recovery rates ranged from 89 to 103% and the relative standard deviations were lower than 13.4%. The applicability of the method was assessed with the analysis of effluent wastewater samples from a wastewater treatment plant located in an agricultural zone of Almería (Spain) and the results indicated the presence of teflubenzuron at mean concentration levels of 11.3 ng L(-1). US-IL-DLLME sample treatment in combination with LC-QqLIT-MS/MS has demonstrated to be a sensitive, selective and efficient method to determine benzoylurea insecticides in wastewaters at ultra-trace levels. PMID:24993054

  12. Targeted analysis of multiple pharmaceuticals, plant toxins and other secondary metabolites in herbal dietary supplements by ultra-high performance liquid chromatography-quadrupole-orbital ion trap mass spectrometry.

    PubMed

    Vaclavik, Lukas; Krynitsky, Alexander J; Rader, Jeanne I

    2014-01-31

    In this study, an ultra-high performance liquid chromatography-quadrupole-orbital ion trap mass spectrometry (UHPLC-Q-orbitrap MS) method was developed and validated for simultaneous determination of 96 pharmaceuticals, plant toxins, and other plant secondary metabolites in herbal dietary supplements. Target analytes were extracted from samples using the QuEChERS (quick easy cheap effective rugged safe) procedure. The instrument was operated in full MS-data dependent tandem mass spectrometry (full MS-dd-MS/MS) acquisition mode which enabled collection of quantitative high resolution (HR) full mass spectral data and confirmatory HR MS/MS data in a single run. The method provided excellent selectivity in both full MS and dd-MS/MS mode. Under optimized collision energy settings, product ion spectra containing both precursor and two or more product ions were obtained for most of the analytes. Limits of detection (LODs) and limits of quantification (LOQs) for the method differed significantly for the examined matrices. LODs≤10μg kg(-1) and LOQs≤50μg kg(-1) were obtained for 48 to 81% of target compounds across five different matrices. With the exception of highly polar analytes, the optimized QuEChERS extraction procedure provided acceptable recoveries in the range 70%-120%. The precision of the method, characterized as the relative standard deviation (RSD, n=5), was ≤25% and ≤18% at spiking concentrations of 50μg kg(-1) and 500μg kg(-1), respectively. Because of variations in matrix effects in extracts of herbal dietary supplements that differed in composition, the method of standard additions and an approach based on dilution of matrix components followed by quantification using solvent standards were applied for quantification. The procedure was used to examine commercial dietary supplements for the 96 analytes of interest. To the best of our knowledge, this is the first report of an integrated analysis and quantification of this wide range of compounds

  13. A strategy for comprehensive identification of sequential constituents using ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometer, application study on chlorogenic acids in Flos Lonicerae Japonicae.

    PubMed

    Zhang, Jia-yu; Wang, Zi-jian; Li, Yun; Liu, Ying; Cai, Wei; Li, Chen; Lu, Jian-qiu; Qiao, Yan-jiang

    2016-01-15

    The analytical methodologies for evaluation of multi-component system in traditional Chinese medicines (TCMs) have been inadequate or unacceptable. As a result, the unclarity of multi-component hinders the sufficient interpretation of their bioactivities. In this paper, an ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap (UPLC-LTQ-Orbitrap)-based strategy focused on the comprehensive identification of TCM sequential constituents was developed. The strategy was characterized by molecular design, multiple ion monitoring (MIM), targeted database hits and mass spectral trees similarity filter (MTSF), and even more isomerism discrimination. It was successfully applied in the HRMS data-acquisition and processing of chlorogenic acids (CGAs) in Flos Lonicerae Japonicae (FLJ), and a total of 115 chromatographic peaks attributed to 18 categories were characterized, allowing a comprehensive revelation of CGAs in FLJ for the first time. This demonstrated that MIM based on molecular design could improve the efficiency to trigger MS/MS fragmentation reactions. Targeted database hits and MTSF searching greatly facilitated the processing of extremely large information data. Besides, the introduction of diagnostic product ions (DPIs) discrimination, ClogP analysis, and molecular simulation, raised the efficiency and accuracy to characterize sequential constituents especially position and geometric isomers. In conclusion, the results expanded our understanding on CGAs in FLJ, and the strategy could be exemplary for future research on the comprehensive identification of sequential constituents in TCMs. Meanwhile, it may propose a novel idea for analyzing sequential constituents, and is promising for quality control and evaluation of TCMs. PMID:26592571

  14. Identification of unsaturated N-acylhomoserine lactones in bacterial isolates of Rhodobacter sphaeroides by liquid chromatography coupled to electrospray ionization-hybrid linear ion trap-Fourier transform ion cyclotron resonance mass spectrometry.

    PubMed

    Cataldi, Tommaso R I; Bianco, Giuliana; Abate, Salvatore; Losito, Ilario

    2011-07-15

    The identification of two unsaturated N-acylhomoserine lactones (AHLs) produced by Rhodobacter sphaeroides bacteria, based on liquid chromatography (LC) coupled to a hybrid quadrupole linear ion trap (LTQ)-Fourier transform ion cyclotron resonance (FTICR) mass spectrometer upon electrospray ionization (ESI), is presented. Besides the confirmation of the signaling molecule already described in the literature, i.e. (Z)-N-tetradec-7-enoyl-homoserine lactone (C(14:1)-HSL), we have discovered the occurrence, at low, yet significant levels, of another monounsaturated compound, C(12:1) -HSL, which may extend the number of small diffusible chemical signals known for R. sphaeroides. Both unsaturated AHLs were identified by high-resolution FTICR mass spectrometry in extracts of bacterial culture media and the occurrence of a C=C bond was assessed upon their conversion into bromohydrins. Collision-induced dissociation (CID) spectra were then collected on the LTQ mass analyzer. A careful comparison of tandem MS spectra of monounsaturated (i.e., C(12:1)-HSL and C(14:1)-HSL) and saturated AHLs (i.e. C(12)-HSL and C(14)-HSL) led to the emphasis of two series of product ions, exhibiting 14 Da spaced m/z ratios. Both series were referred to progressive fragmentations at the aliphatic end of the AHL acyl chains, followed by neutral losses of terminal alkenes (i.e. CH(2)=CH(CH(2))(n)H). In particular, the series located at the higher end of the explored m/z range (>200 Da), observed only for monounsaturated species, enabled the location of the C=C bond between carbons 7 and 8 of the acyl chain. PMID:21638357

  15. Microfabricated linear Paul-Straubel ion trap

    DOEpatents

    Mangan, Michael A.; Blain, Matthew G.; Tigges, Chris P.; Linker, Kevin L.

    2011-04-19

    An array of microfabricated linear Paul-Straubel ion traps can be used for mass spectrometric applications. Each ion trap comprises two parallel inner RF electrodes and two parallel outer DC control electrodes symmetric about a central trap axis and suspended over an opening in a substrate. Neighboring ion traps in the array can share a common outer DC control electrode. The ions confined transversely by an RF quadrupole electric field potential well on the ion trap axis. The array can trap a wide array of ions.

  16. Thermal modulation for gas chromatography

    NASA Technical Reports Server (NTRS)

    Hasselbrink, Ernest F. (Inventor); Libardoni, Mark (Inventor); Stewart, Kristine (Inventor); Waite, J. Hunter (Inventor); Block, Bruce P. (Inventor); Sacks, Richard D. (Inventor)

    2007-01-01

    A thermal modulator device for gas chromatography and associated methods. The thermal modulator device includes a recirculating fluid cooling member, an electrically conductive capillary in direct thermal contact with the cooling member, and a power supply electrically coupled to the capillary and operable for controlled resistive heating of the capillary. The capillary can include more than one separate thermally modulated sections.

  17. Thermal modulation for gas chromatography

    NASA Technical Reports Server (NTRS)

    Hasselbrink, Ernest F. (Inventor); Libardoni, Mark (Inventor); Stewart, Kristine (Inventor); Waite, J. Hunter (Inventor); Block, Bruce P. (Inventor); Sacks, Richard D. (Inventor)

    2007-01-01

    A thermal modulator device for gas chromatography and associated methods. The thermal modulator device includes a cooling member, an electrically conductive capillary in direct thermal contact with the cooling member, and a power supply electrically coupled to the capillary and operable for controlled resistive heating of the capillary.

  18. Automated gas chromatography

    DOEpatents

    Mowry, Curtis D.; Blair, Dianna S.; Rodacy, Philip J.; Reber, Stephen D.

    1999-01-01

    An apparatus and process for the continuous, near real-time monitoring of low-level concentrations of organic compounds in a liquid, and, more particularly, a water stream. A small liquid volume of flow from a liquid process stream containing organic compounds is diverted by an automated process to a heated vaporization capillary where the liquid volume is vaporized to a gas that flows to an automated gas chromatograph separation column to chromatographically separate the organic compounds. Organic compounds are detected and the information transmitted to a control system for use in process control. Concentrations of organic compounds less than one part per million are detected in less than one minute.

  19. Automated gas chromatography

    DOEpatents

    Mowry, C.D.; Blair, D.S.; Rodacy, P.J.; Reber, S.D.

    1999-07-13

    An apparatus and process for the continuous, near real-time monitoring of low-level concentrations of organic compounds in a liquid, and, more particularly, a water stream. A small liquid volume of flow from a liquid process stream containing organic compounds is diverted by an automated process to a heated vaporization capillary where the liquid volume is vaporized to a gas that flows to an automated gas chromatograph separation column to chromatographically separate the organic compounds. Organic compounds are detected and the information transmitted to a control system for use in process control. Concentrations of organic compounds less than one part per million are detected in less than one minute. 7 figs.

  20. On-Line Derivatization Gas Chromatography Ion Trap Mass Spectrometry for Determination of Endocrine Disruptors in Surface Water

    SciTech Connect

    Tzing, Shin-Hwa; Chang, Jia-Yaw; Ling, Yong-Chien

    2004-03-31

    A method has been developed for the determination of endocrine disruptors (EDs) (containing hydroxyl groups) in surface water from different sources. The surface water samples from different sites including school and local dormitory sewage effluents, lake water and river water were collected and analyzed. In this method, the pretreated sample is directly analyzed by GC-MS using on-line derivatization, where tetramethylammonium hydroxide (TMA-OH) was used as the derivatizing agent. Use of large-volume direct sample introduction (DSI) and co-injection of the sample and TMAOH avoids external contaminations as observed in conventional derivatization protocols. Additionally, the use of chemical ionization (CI) and CI-MS/MS could enable detection of EDs at lower concentrations and reduce the matrices' interference thereby enhancing detection sensitivity of EDs for quantification. In this work, the use of dichloromethane as CI reagent for EDs is reported for the first time and could detect EDs to concentrations as low as 0.5 pg/mL. The recovery ranged from 74 to 112 % and the relative standard derivations for replicate analyses ranged from 5 to 17 %. We hope that this method will be applicable for routine analysis of EDs with hydroxyl functional groups.

  1. Comparison of Data Acquisition Strategies on Quadrupole Ion Trap Instrumentation for Shotgun Proteomics

    PubMed Central

    Canterbury, Jesse D.; Merrihew, Gennifer E.; Goodlett, David R.; MacCoss, Michael J.; Shaffer, Scott A.

    2015-01-01

    A common strategy in mass spectrometry analyses of complex protein mixtures is to digest the proteins to peptides, separate the peptides by microcapillary liquid chromatography and collect tandem mass spectra (MS/MS) on the eluting, complex peptide mixtures, a process commonly termed “shotgun proteomics”. For years, the most common way of data collection was via data-dependent acquisition (DDA), a process driven by an automated instrument control routine that directs MS/MS acquisition from the highest abundant signals to the lowest, a process often leaving lower abundant signals unanalyzed and therefore unidentified in the experiment. Advances in both instrumentation duty cycle and sensitivity allow DDA to probe to lower peptide abundance and therefore enable mapping proteomes to a more significant depth. An alternative to acquiring data by DDA is by data-independent acquisition (DIA), in which a specified range in m/z is fragmented without regard to prioritization of a precursor ion or its relative abundance in the mass spectrum. As a consequence, DIA acquisition potentially offers more comprehensive analysis of peptides than DDA and in principle can yield tandem mass spectra of all ionized molecules following their conversion to the gas-phase. In this work, we evaluate both DDA and DIA on three different linear ion trap instruments: an LTQ, an LTQ modified in-house with an electrodynamic ion funnel, and an LTQ-Velos. These instruments were chosen as they are representative of both older (LTQ) and newer (LTQ-Velos) ion trap designs i.e., linear ion trap and dual ion traps, respectively, and allow direct comparison of peptide identification using both DDA and DIA analysis. Further, as the LTQ-Velos has an improved “S-lens” ion guide in the high-pressure region to improve ion flux, we found it logical to determine if the former LTQ model could be leveraged by improving sensitivity by modifying with an electrodynamic ion guide of significantly different

  2. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction coupled with liquid chromatography-quadrupole-linear ion trap-mass spectrometry for simultaneous analysis of pharmaceuticals in wastewaters.

    PubMed

    Parrilla Vázquez, M M; Parrilla Vázquez, P; Martínez Galera, M; Gil García, M D; Uclés, A

    2013-05-24

    A simple, rapid, low environmental toxicity and sensitive ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (US-IL-DLLME) procedure was developed for the extraction of nine pharmaceuticals (paracetamol, metoprolol, bisoprolol, betaxolol, ketoprofen, naproxen, ibuprofen, flufenamic acid and tolfenamic acid) in wastewater, and their determination using high-performance liquid chromatography with a hybrid triple quadrupole-linear ion trap-mass spectrometer (LC-QqLIT-MS). The IL 1-octyl-3-methylimidazolium hexafluorophosphate ([C8MIM][PF6]) and acetonitrile (ACN) were used as extraction and disperser solvent, respectively, for the DLLME procedure, instead of using toxic chlorinated solvent. The factors affecting the extraction efficiency, such as the type and volume of ionic liquid, type and volume of disperser solvent, cooling in ice-water, sonication time, centrifuging time, sample pH and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution using a small volume of disperser solvent (0.5mL of acetonitrile), which increased the extraction efficiency and reduced the equilibrium time. A slight increase in the recoveries of pharmaceuticals was observed when an ice-water bath extraction step was included in the analytical procedure. In this way, enrichment factors between 255 and 340 were obtained. Data acquisition in selected reaction monitoring mode (SRM), allowed the simultaneous identification and quantification of the analytes using two transitions (SRM1 and SRM2). Additionally, the information dependent acquisition (IDA) scan was performed to carry out the identification of those analytes whose second transition was absent or was present at low intensity, also providing extra confirmation for the other analytes. The optimized US-IL-DLLME-LC-QqLIT-MS method showed a good precision level, with relative standard deviation values between 1.1% and 11.3%. Limits of

  3. A comprehensive library-based, automated screening procedure for 46 synthetic cannabinoids in serum employing liquid chromatography-quadrupole ion trap mass spectrometry with high-temperature electrospray ionization.

    PubMed

    Huppertz, Laura M; Kneisel, Stefan; Auwärter, Volker; Kempf, Jürgen

    2014-02-01

    Considering the vast variety of synthetic cannabinoids and herbal mixtures - commonly known as 'Spice' or 'K2' - on the market and the resulting increase of severe intoxications related to their consumption, there is a need in clinical and forensic toxicology for comprehensive up-to-date screening methods. The focus of this project aimed at developing and implementing an automated screening procedure for the detection of synthetic cannabinoids in serum using a liquid chromatography-ion trap-MS (LC-MS(n)) system and a spectra library-based approach, currently including 46 synthetic cannabinoids and 8 isotope labelled analogues. In the process of method development, a high-temperature ESI source (IonBooster(TM), Bruker Daltonik) and its effects on the ionization efficiency of the investigated synthetic cannabinoids were evaluated and compared to a conventional ESI source. Despite their structural diversity, all investigated synthetic cannabinoids benefitted from high-temperature ionization by showing remarkably higher MS intensities compared to conventional ESI. The employed search algorithm matches retention time, MS and MS(2)/MS(3) spectra. With the utilization of the ionBooster source, limits for the automated detection comparable to cut-off values of routine MRM methods were achieved for the majority of analytes. Even compounds not identified when using a conventional ESI source were detected using the ionBooster-source. LODs in serum range from 0.1 ng/ml to 0.5 ng/ml. The use of parent compounds as analytical targets offers the possibility of instantly adding new emerging compounds to the library and immediately applying the updated method to serum samples, allowing the rapid adaptation of the screening method to ongoing forensic or clinical requirements. The presented approach can also be applied to other specimens, such as oral fluid or hair, and herbal mixtures and was successfully applied to authentic serum samples. Quantitative MRM results of samples with

  4. Three-Rod Linear Ion Traps

    NASA Technical Reports Server (NTRS)

    Janik, Gary R.; Prestage, John D.; Maleki, Lutfollah

    1993-01-01

    Three-parallel-rod electrode structures proposed for use in linear ion traps and possibly for electrostatic levitation of macroscopic particles. Provides wider viewing angle because they confine ions in regions outside rod-electrode structures.

  5. Improved Linear-Ion-Trap Frequency Standard

    NASA Technical Reports Server (NTRS)

    Prestage, John D.

    1995-01-01

    Improved design concept for linear-ion-trap (LIT) frequency-standard apparatus proposed. Apparatus contains lengthened linear ion trap, and ions processed alternately in two regions: ions prepared in upper region of trap, then transported to lower region for exposure to microwave radiation, then returned to upper region for optical interrogation. Improved design intended to increase long-term frequency stability of apparatus while reducing size, mass, and cost.

  6. Experimental investigation of planar ion traps

    SciTech Connect

    Pearson, C. E.; Leibrandt, D. R.; Bakr, W. S.; Mallard, W. J.; Brown, K. R.; Chuang, I. L.

    2006-03-15

    Chiaverini et al. [Quantum Inf. Comput. 5, 419 (2005)] recently suggested a linear Paul trap geometry for ion-trap quantum computation that places all of the electrodes in a plane. Such planar ion traps are compatible with modern semiconductor fabrication techniques and can be scaled to make compact, many-zone traps. In this paper we present an experimental realization of planar ion traps using electrodes on a printed circuit board to trap linear chains of tens of charged particles of 0.44 {mu}m diameter in a vacuum of 15 Pa (10{sup -1} torr). With these traps we address concerns about the low trap depth of planar ion traps and develop control electrode layouts for moving ions between trap zones without facing some of the technical difficulties involved in an atomic ion-trap experiment. Specifically, we use a trap with 36 zones (77 electrodes) arranged in a cross to demonstrate loading from a traditional four-rod linear Paul trap, linear ion movement, splitting and joining of ion chains, and movement of ions through intersections. We further propose an additional dc-biased electrode above the trap which increases the trap depth dramatically, and a planar ion-trap geometry that generates a two-dimensional lattice of point Paul traps.

  7. Single Ion Trapping for the Enriched Xenon Observatory

    SciTech Connect

    Waldman, Samuel J.; /Stanford U., Phys. Dept. /SLAC

    2006-03-28

    In the last decade, a variety of neutrino oscillation experiments have established that there is a mass difference between neutrino flavors, without determining the absolute neutrino mass scale. The Enriched Xenon Observatory for neutrinoless double beta decay (EXO) will search for the rare decays of xenon to determine the absolute value of the neutrino mass. The experiment uses a novel technique to minimize backgrounds, identifying the decay daughter product in real time using single ion spectroscopy. Here, we describe single ion trapping and spectroscopy compatible with the EXO detector. We extend the technique of single ion trapping in ultrahigh vacuum to trapping in xenon gas. With this technique, EXO will achieve a neutrino mass sensitivity of {approx_equal} .010 eV.

  8. Active stabilization of ion trap radiofrequency potentials

    NASA Astrophysics Data System (ADS)

    Johnson, K. G.; Wong-Campos, J. D.; Restelli, A.; Landsman, K. A.; Neyenhuis, B.; Mizrahi, J.; Monroe, C.

    2016-05-01

    We actively stabilize the harmonic oscillation frequency of a laser-cooled atomic ion confined in a radiofrequency (rf) Paul trap by sampling and rectifying the high voltage rf applied to the trap electrodes. We are able to stabilize the 1 MHz atomic oscillation frequency to be better than 10 Hz or 10 ppm. This represents a suppression of ambient noise on the rf circuit by 34 dB. This technique could impact the sensitivity of ion trap mass spectrometry and the fidelity of quantum operations in ion trap quantum information applications.

  9. Finnigan ion trap mass spectrometer detection limits and thermal energy analyzer interface status report and present capabilities

    SciTech Connect

    Alcaraz, A.; Andresen, B.; Martin, W.

    1990-10-18

    A new Finnigan ion trap mass spectrometer was purchased and installed at LLNL. Over a period of several months the instrument was tested under a variety of conditions utilizing a capillary gas chromatography interface which allowed separated organic compounds to be carried directly into the ion source of the mass spectrometer. This direct interface allowed maximum analytical sensitivity. A variety of critical tests were performed in order to optimize the sensitivity of the system under a variety of analysis conditions. These tests altered the critical time cycles of the ionization, ion trapping, and detection. Various carrier gas pressures were also employed in order to ascertain the overall sensitivity of the instrument. In addition we have also interfaced a thermal energy analyzer (TEA) to the gas chromatograph in order to simultaneously detect volatile nitrogen containing compounds while mass spectral data is being acquired. This is the first application at this laboratory of simultaneous ultra-trace detections while utilizing two orthogonal analytical techniques. In particular, explosive-related compound and/or residues are of interest to the general community in water, soil and gas sampler. In this paper are highlighted a few examples of the analytical power of this new GC-TEA-ITMS technology.

  10. Space-charge effects in Penning ion traps

    NASA Astrophysics Data System (ADS)

    Porobić, T.; Beck, M.; Breitenfeldt, M.; Couratin, C.; Finlay, P.; Knecht, A.; Fabian, X.; Friedag, P.; Fléchard, X.; Liénard, E.; Ban, G.; Zákoucký, D.; Soti, G.; Van Gorp, S.; Weinheimer, Ch.; Wursten, E.; Severijns, N.

    2015-06-01

    The influence of space-charge on ion cyclotron resonances and magnetron eigenfrequency in a gas-filled Penning ion trap has been investigated. Off-line measurements with K39+ using the cooling trap of the WITCH retardation spectrometer-based setup at ISOLDE/CERN were performed. Experimental ion cyclotron resonances were compared with ab initio Coulomb simulations and found to be in agreement. As an important systematic effect of the WITCH experiment, the magnetron eigenfrequency of the ion cloud was studied under increasing space-charge conditions. Finally, the helium buffer gas pressure in the Penning trap was determined by comparing experimental cooling rates with simulations.

  11. Simultaneous quantification of poly-dispersed anionic, amphoteric and nonionic surfactants in simulated wastewater samples using C18 high-performance liquid chromatography-quadrupole ion-trap mass spectrometry

    NASA Technical Reports Server (NTRS)

    Levine, Lanfang H.; Garland, Jay L.; Johnson, Jodie V.

    2005-01-01

    This paper describes the development of a guantitative method for direct and simultaneous determination of three frequently encountered surfactants, amphoteric (cocoamphoacetate, CAA), anionic (sodium laureth sulfate, SLES), and nonionic (alcohol ethoxylate, AE) using a reversed-phase C18 HPLC coupled with an ESI ion-trap mass spectrometer (MS). Chemical composition, ionization characteristics and fragmentation pathways of the surfactants are presented. Positive ESI was effective for all three surfactants in agueous methanol buffered with ammonium acetate. The method enables rapid determinations in small sample volumes containing inorganic salts (up to 3.5 g L(-1)) and multiple classes of surfactants with high specificity by applying surfactant specific tandem mass spectrometric strategies. It has dynamic linear ranges of 2-60, 1.5-40, 0.8-56 mg L(-1) with R2 egual or greater than 0.999, 0.98 and 0.999 (10 microL injection) for CAA, SLES, and AE, respectively.

  12. Real-time air monitoring of mustard gas and Lewisite 1 by detecting their in-line reaction products by atmospheric pressure chemical ionization ion trap tandem mass spectrometry with counterflow ion introduction.

    PubMed

    Okumura, Akihiko; Takada, Yasuaki; Watanabe, Susumu; Hashimoto, Hiroaki; Ezawa, Naoya; Seto, Yasuo; Sekiguchi, Hiroshi; Maruko, Hisashi; Takayama, Yasuo; Sekioka, Ryoji; Yamaguchi, Shintaro; Kishi, Shintaro; Satoh, Takafumi; Kondo, Tomohide; Nagashima, Hisayuki; Nagoya, Tomoki

    2015-01-20

    A new method enabling sensitive real-time air monitoring of highly reactive chemical warfare agents, namely, mustard gas (HD) and Lewisite 1 (L1), by detecting ions of their in-line reaction products instead of intact agents, is proposed. The method is based on corona discharge-initiated atmospheric pressure chemical ionization coupled with ion trap tandem mass spectrometry (MS(n)) via counterflow ion introduction. Therefore, it allows for highly sensitive and specific real-time detection of a broad range of airborne compounds. In-line chemical reactions, ionization reactions, and ion fragmentations of these agents were investigated. Mustard gas is oxygenated in small quantity by reactive oxygen species generated in the corona discharge. With increasing air humidity, the MS(2) signal intensity of protonated molecules of mono-oxygenated HD decreases but exceeds that of dominantly existing intact HD. This result can be explained in view of proton affinity. Lewisite 1 is hydrolyzed and oxidized. As the humidity increases from zero, the signal of the final product, namely, didechlorinated, dihydroxylated, and mono-oxygenated L1, quickly increases and reaches a plateau, giving the highest MS(2) and MS(3) signals among those of L1 and its reaction products. The addition of minimal moisture gives the highest signal intensity, even under low humidity. The method was demonstrated to provide sufficient analytical performance to meet the requirements concerning hygienic management and counter-terrorism. It will be the first practical method, in view of sensitivity and specificity, for real-time air monitoring of HD and L1 without sample pretreatment. PMID:25553788

  13. Multielement detector for gas chromatography

    SciTech Connect

    Sklarew, D.S.; Evans, J.C.; Olsen, K.B.

    1988-11-01

    This report describes the results of a study to improve the capabilities of a gas chromatography-microwave-induced plasma (GC- MIP) detector system, determine the feasibility of empirical formula determination for simple mixtures containing elements of interest to fossil fuel analysis and, subsequently, explore applications for analysis of the complex mixtures associated with fossil fuels. The results of this study indicate that the GC-MIP system is useful as a specific-element detector that provides excellent elemental specificity for a number of elements of interest to the analysis of fossil fuels. It has reasonably good sensitivity for carbon, hydrogen, sulfur, and nickel, and better sensitivity for chlorine and fluorine. Sensitivity is poor for nitrogen and oxygen, however, probably because of undetected leaks or erosion of the plasma tube. The GC-MIP can also provide stoichiometric information about components of simple mixtures. If this powerful technique is to be available for complex mixtures, it will be necessary to greatly simplify the chromatograms by chemical fractionation. 38 refs., 46 figs., 16 tabs.

  14. Mars Organic Molecule Analyzer (MOMA) Mass Spectrometer Flight Model and Future Ion Trap-Based Planetary Instruments

    NASA Astrophysics Data System (ADS)

    Brinckerhoff, W. B.; van Amerom, F. H. W.; Danell, R.; Pinnick, V. T.; Arevalo, R. D., Jr.; Li, X.; Grubisic, A.; Getty, S.; Hovmand, L.; Mahaffy, P. R.

    2015-12-01

    The Mars Organic Molecule Analyzer (MOMA) investigation on the 2018 ExoMars rover will examine the chemical composition of samples acquired from depths of up to two meters below the martian surface, where organics may be protected from radiative and oxidative degradation. MOMA combines pyrolysis gas chromatography mass spectrometry (GCMS) of bulk powder samples and Mars ambient laser desorption mass spectrometry (LDMS) surface analysis, using a single ion trap MS. This dual source design enables MOMA to detect compounds over a wide range of molecular weights and volatilities. The structure of any detected organics may be further examined using MOMA's tandem mass spectrometry (MS/MS) mode. The flight model (FM) ion trap sensor and electronics have been assembled under the extremely clean and sterile conditions required by ExoMars, and have met or exceeded all performance specifications during initial functional tests. After Mars ambient thermal cycling and calibration, the FM will be delivered as a subsystem of MOMA to rover integration in mid-2016. There MOMA will join complementary rover instruments such as the Raman and MicrOmega spectrometers designed to analyze common drill samples. Following the MOMA design, linear ion trap mass spectrometer (LITMS)-based instruments are under development for future missions. LITMS adds enhanced capabilities such as precision (point-by-point) analysis of drill cores, negative ion detection, a wider mass range, and higher temperature pyrolysis with precision evolved gas analysis, while remaining highly compact and robust. Each of the capabilities of LITMS has been demonstrated on breadboard hardware. The next phase will realize an end-to-end brassboard at flight scale that will meet stringent technology readiness level (TRL) 6 criteria, indicating readiness for development toward missions to Mars, comets, asteroids, outer solar system moons, and beyond.

  15. Performance characteristics of an automated gas chromatograph-ion trap mass spectrometer system used for the 1995 Southern Oxidants Study field investigation in Nashville, Tennessee

    NASA Astrophysics Data System (ADS)

    Daughtrey, E. Hunter; Adams, Jeffrey R.; Oliver, Karen D.; Kronmiller, Keith G.; McClenny, William A.

    1998-09-01

    A trailer-deployed automated gas chromatograph-mass spectrometer (autoGC-MS) system capable of making continuous hourly measurements was used to determine volatile organic compounds (VOCs) in ambient air at New Hendersonville, Tennessee, and Research Triangle Park, North Carolina, in 1995. The system configuration, including the autoGC-MS, trailer and transfer line, siting, and sampling plan and schedule, is described. The autoGC-MS system employs a pair of matched sorbent traps to allow simultaneous sampling and desorption. Desorption is followed by Stirling engine cryofocusing and subsequent GC separation and mass spectral identification and quantification. Quality control measurements described include evaluating precision and accuracy of replicate analyses of independently supplied audit and round-robin canisters and determining the completeness of the data sets taken in Tennessee. Data quality objectives for precision (±10%) and accuracy (±20%) of 10- to 20-ppbv audit canisters and a completeness of >75% data capture were met. Quality assurance measures used in reviewing the data set include retention time stability, calibration checks, frequency distribution checks, and checks of the mass spectra. Special procedures and tests were used to minimize sorbent trap artifacts, to verify the quality of a standard prepared in our laboratory, and to prove the integrity of the insulated, heated transfer line. A rigorous determination of total system blank concentration levels using humidified scientific air spiked with ozone allowed estimation of method detection limits, ranging from 0.01 to 1.0 ppb C, for most of the 100 target compounds, which were a composite list of the target compounds for the Photochemical Assessment Monitoring Station network, those for Environmental Protection Agency method TO-14, and selected oxygenated VOCs.

  16. Linear Ion Traps in Space: The Mars Organic Molecule Analyzer (MOMA) Instrument and Beyond

    NASA Astrophysics Data System (ADS)

    Arevalo, Ricardo; Brinckerhoff, William; Mahaffy, Paul; van Amerom, Friso; Danell, Ryan; Pinnick, Veronica; Li, Xiang; Hovmand, Lars; Getty, Stephanie; Grubisic, Andrej; Goesmann, Fred; Cottin, Hervé

    2015-11-01

    Historically, quadrupole mass spectrometer (QMS) instruments have been used to explore a wide survey of planetary targets in our solar system, from Venus (Pioneer Venus) to Saturn (Cassini-Huygens). However, linear ion trap (LIT) mass spectrometers have found a niche as smaller, versatile alternatives to traditional quadrupole analyzers.The core astrobiological experiment of ESA’s ExoMars Program is the Mars Organic Molecule Analyzer (MOMA) onboard the ExoMars 2018 rover. The MOMA instrument is centered on a linear (or 2-D) ion trap mass spectrometer. As opposed to 3-D traps, LIT-based instruments accommodate two symmetrical ion injection pathways, enabling two complementary ion sources to be used. In the case of MOMA, these two analytical approaches are laser desorption mass spectrometry (LDMS) at Mars ambient pressures, and traditional gas chromatography mass spectrometry (GCMS). The LIT analyzer employed by MOMA also offers: higher ion capacity compared to a 3-D trap of the same volume; redundant detection subassemblies for extended lifetime; and, a link to heritage QMS designs and assembly logistics. The MOMA engineering test unit (ETU) has demonstrated the detection of organics in the presence of wt.%-levels of perchlorate, effective ion enhancement via stored waveform inverse Fourier transform (SWIFT), and derivation of structural information through tandem mass spectrometry (MS/MS).A more progressive linear ion trap mass spectrometer (LITMS), funded by the NASA ROSES MatISSE Program, is being developed at NASA GSFC and promises to augment the capabilities of the MOMA instrument by way of: an expanded mass range (i.e., 20 - 2000 Da); detection of both positive and negative ions; spatially resolved (<1 mm) characterization of individual rock core layers; and, evolved gas analysis and GCMS with pyrolysis up to 1300° C (enabling breakdown of refractory phases). The Advanced Resolution Organic Molecule Analyzer (AROMA) instrument, being developed through NASA

  17. Miniaturized Linear Wire Ion Trap Mass Analyzer.

    PubMed

    Wu, Qinghao; Li, Ailin; Tian, Yuan; Zare, Richard N; Austin, Daniel E

    2016-08-01

    We report a linear ion trap (LIT) in which the electric field is formed by fine wires held under tension and accurately positioned using holes drilled in two end plates made of plastic. The coordinates of the hole positions were optimized in simulation. The stability diagram and mass spectra using boundary ejection were compared between simulation and experiment and good agreement was found. The mass spectra from experiments show peak widths (fwhm) in units of mass-to-charge of around 0.38 Th using a scan rate of 3830 Th/s. The limits of detection are 137 ppbv and 401 ppbv for benzene and toluene, respectively. Different sizes of the wire ion trap can be easily fabricated by drilling holes in scaled positions. Other distinguishing features, such as high ion and photon transmission, low capacitance, high tolerance to mechanical and assembly error, and low weight, are discussed. PMID:27373557

  18. Ion trap in a semiconductor chip

    NASA Astrophysics Data System (ADS)

    Stick, D.; Hensinger, W. K.; Olmschenk, S.; Madsen, M. J.; Schwab, K.; Monroe, C.

    2006-01-01

    The electromagnetic manipulation of isolated atoms has led to many advances in physics, from laser cooling and Bose-Einstein condensation of cold gases to the precise quantum control of individual atomic ions. Work on miniaturizing electromagnetic traps to the micrometre scale promises even higher levels of control and reliability. Compared with `chip traps' for confining neutral atoms, ion traps with similar dimensions and power dissipation offer much higher confinement forces and allow unparalleled control at the single-atom level. Moreover, ion microtraps are of great interest in the development of miniature mass-spectrometer arrays, compact atomic clocks and, most notably, large-scale quantum information processors. Here we report the operation of a micrometre-scale ion trap, fabricated on a monolithic chip using semiconductor micro-electromechanical systems (MEMS) technology. We confine, laser cool and measure heating of a single 111Cd+ ion in an integrated radiofrequency trap etched from a doped gallium-arsenide heterostructure.

  19. Experiments in Planar Multipole Ion Traps

    NASA Astrophysics Data System (ADS)

    Clark, Rob; Burke, Timothy; Green, Dylan

    2016-05-01

    We present the design and demonstration of multipole ion traps based on concentric rings. We have developed both surface-electrode and layered planar trap designs which enable one to null the quadratic term in the electric potential to a high degree. Experiments demonstrating frequency upconversion of an applied signal demonstrate the nonlinear dynamics present in the trap. Applications include quantum chaos, ultracold chemistry, and, potentially, mass spectrometry. We acknowledge support from the Research Corporation for Science Advancement and from The Citadel Foundation.

  20. Ionization-based detectors for gas chromatography.

    PubMed

    Poole, Colin F

    2015-11-20

    The gas phase ionization detectors are the most widely used detectors for gas chromatography. The column and makeup gases commonly used in gas chromatography are near perfect insulators. This facilitates the detection of a minute number of charge carriers facilitating the use of ionization mechanisms of low efficiency while providing high sensitivity. The main ionization mechanism discussed in this report are combustion in a hydrogen diffusion flame (flame ionization detector), surface ionization in a plasma (thermionic ionization detector), photon ionization (photoionization detector and pulsed discharge helium ionization detector), attachment of thermal electrons (electron-capture detector), and ionization by collision with metastable helium species (helium ionization detector). The design, response characteristics, response mechanism, and suitability for fast gas chromatography are the main features summarized in this report. Mass spectrometric detection and atomic emission detection, which could be considered as ionization detectors of a more sophisticated and complex design, are not discussed in this report. PMID:25757823

  1. Unknown exposures: gaps in basic characterization addressed with person-portable gas chromatography-mass spectrometry instrumentation.

    PubMed

    Smith, Philip A; Roe, Marc T A; Sadowski, Charles; Lee, Edgar D

    2011-03-01

    A newly developed person-portable gas chromatography-mass spectrometry (GC-MS) system was used to analyze several solvent standards, contact cement, paint thinner, and polychlorinated biphenyl samples. Passive solid phase microextraction sampling and fast chromatography with a resistively heated low thermal mass GC column were used. Results (combined sampling and analysis) were obtained in <2 min for solvent, contact cement, and paint thinner samples, and in <13 min for the polychlorinated biphenyl sample. Mass spectra produced by the small toroidal ion trap detector used were similar to those produced with heavily used transmission quadrupole mass spectrometers for polychlorinated biphenyl compounds, simple alkanes, and cycloalknes, while mass spectra for benzene and the ketone compounds analyzed showed evidence for ion/molecule reactions in the ion trap. For one of the contact cement samples analyzed, no evidence was found to indicate the presence of n-hexane, although the relevant material safety data sheet listed this ingredient. Specific chemical constituents corresponding to a potentially wide range of petroleum distillate compounds were identifiable from GC-MS analyses. The possibility for an improved basic characterization step in the exposure assessment process exists with the availability of fast, person-portable GC-MS, although work is needed to further refine this tool and understand the best ways it may be used. PMID:21318921

  2. Rapid screening of drugs of abuse in human urine by high-performance liquid chromatography coupled with high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometry.

    PubMed

    Li, Xiaowen; Shen, Baohua; Jiang, Zheng; Huang, Yi; Zhuo, Xianyi

    2013-08-01

    A novel analytical toxicology method has been developed for the analysis of drugs of abuse in human urine by using a high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS). This method allows for the detection of different drugs of abuse, including amphetamines, cocaine, opiate alkaloids, cannabinoids, hallucinogens and their metabolites. After solid-phase extraction with Oasis HLB cartridges, spiked urine samples were analysed by HPLC/LTQ-Orbitrap-MS using an electrospray interface in positive ionisation mode, with resolving power of 30,000 full width at half maximum (FWHM). Gradient elution off of a Hypersil Gold PFP column (50mm×2.1mm) allowed to resolve 65 target compounds and 3 internal standards in a total chromatographic run time of 20min. Validation of this method consisted of confirmation of identity, selectivity, linearity, limit of detection (LOD), lowest limits of quantification (LLOQ), accuracy, precision, extraction recovery and matrix effect. The regression coefficients (r(2)) for the calibration curves (LLOQ - 100ng/mL) in the study were ≥0.99. The LODs for 65 validated compounds were better than 5ng/ml except for 4 compounds. The relative standard deviation (RSD), which was used to estimate repeatability at three concentrations, was always less than 15%. The recovery of extraction and matrix effects were above 50 and 70%, respectively. Mass accuracy was always better than 2ppm, corresponding to a maximum mass error of 0.8 millimass units (mmu). The accurate masses of characteristic fragments were obtained by collisional experiments for a more reliable identification of the analytes. Automated data analysis and reporting were performed using ToxID software with an exact mass database. This procedure was then successfully applied to analyse drugs of abuse in a real urine sample from subject who was assumed to be drug addict. PMID:23838299

  3. Simultaneous determination of triazine herbicides in rice by high-performance liquid chromatography coupled with high resolution and high mass accuracy hybrid linear ion trap-orbitrap mass spectrometry.

    PubMed

    Mou, Ren-Xiang; Chen, Ming-Xue; Cao, Zhao-Yun; Zhu, Zhi-Wei

    2011-11-01

    A method was developed for the simultaneous determination of 10 triazine herbicides (cyanazine, simazine, simetryn, metribuzin, atrazine, ametryn, terbuthylazine, prometryn, terbutryn, and dimethametryn) in rice samples by high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer. After extraction with acetonitrile and evaporation, the herbicides were redissolved in n-hexane and purified on a Florisil solid-phase extraction column. All compounds were separated within 12 min, producing more than 11 data points for each herbicide and high mass accuracy quantified ions which the mass errors of absolute value were less than 1.9 ppm in pure solution and 2.1 ppm in the matrix-matched standards solution. The method was validated in terms of the limits of detection and the limits of quantification. The linearity was satisfactory, with a correlation coefficient of >0.9975. Precision and recovery studies were evaluated at three concentration levels for Japonica, Indica, and Glutinous rice matrix. The mean recoveries obtained for all analytes in spiked Xiushui 03, Liangyoupeijiu, and Taihunuo rice samples were 83.3-99.0%, 82.0-99.7%, and 84.2-99.4%, respectively, with relative standard deviation in range 1.7-10.6%, 1.2-10.7%, and 1.9-11.6% for spiked rice samples, respectively. The intra-day precision (n=5) for the 10 herbicides in rice samples spiked at an intermediate level was between 2.8% and 7.9%, and the inter-day precision over 10 days (n=10) was between 5.5% and 15.9%. PMID:21995922

  4. Rapid, high performance method for the determination of vitamin K(1), menaquinone-4 and vitamin K(1) 2,3-epoxide in human serum and plasma using liquid chromatography-hybrid quadrupole linear ion trap mass spectrometry.

    PubMed

    Gentili, Alessandra; Cafolla, Arturo; Gasperi, Tecla; Bellante, Simona; Caretti, Fulvia; Curini, Roberta; Fernández, Virginia Pérez

    2014-04-18

    Unlike the other fat-soluble vitamins, vitamin K circulates in the human bloodstream at very low levels because of a low intake in the diet. Mammals have developed an efficient recycling system, known as vitamin K-epoxide cycle, which involve quinone, hydroquinone and epoxide forms of the vitamin. Phylloquinone (K(1)) is the main homologue, while menaquinone-4 (MK-4) is both a member of the vitamin K(2) family and metabolite of K(1) in extra-hepatic tissues. Notwithstanding the recent advances, many aspects of the complex vitamin K physiology still remain to be investigated. Therefore, there is a critical need to develop more reliable analytical methods for determining the vitamin K and its metabolites in biological fluids and tissues. Nevertheless, relatively low concentrations, unavailability of some authentic standards and occurrence of interfering lipids make this a challenging task. The method proposed in the present paper can directly and accurately estimate K(1), K(1) 2,3-epoxide (K(1)O), and MK-4 in human serum and plasma at concentrations in the ng/L-μg/L range, using labelled internal standards and a quadrupole linear ion trap instrument operated in multiple reaction monitoring (MRM) mode. High sensitivity was achieved by removing signal "endogenous suppressors" and making the composition of the non-aqueous mobile phase suitable to support the positive atmospheric pressure chemical ionization of the analytes. An excellent selectivity resulted from the combination of some factors: the MRM acquisition, the adoption of an identification point system, an extraction optimized to remove most of the lipids and a tandem-C18 column-system necessary to separate isobaric interferences from analytes. The method was validated according to the Food and Drug Administration (FDA) guidelines and its accuracy was assessed by analysing 9 samples from the Vitamin K External Quality Assessment Scheme (KEQAS). Its feasibility in evaluating vitamin K status in human serum was

  5. Monitoring Trace Contaminants in Air Via Ion Trap Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Palmer, Peter T.; Karr, Dane; Pearson, Richard; Valero, Gustavo; Wong, Carla

    1995-01-01

    Recent passage of the Clean Air Act with its stricter regulation of toxic gas emissions, and the ever-growing number of applications which require faster turnaround times between sampling and analysis are two major factors which are helping to drive the development of new instrument technologies for in-situ, on-line, real-time monitoring. The ion trap, with its small size, excellent sensitivity, and tandem mass spectrometry capability is a rapidly evolving technology which is well-suited for these applications. In this paper, we describe the use of a commercial ion trap instrument for monitoring trace levels of chlorofluorocarbons (CFCs) and volatile organic compounds (VOCs) in air. A number of sample introduction devices including a direct transfer line interface, short column GC, and a cryotrapping interface are employed to achieve increasing levels of sensitivity. MS, MS/MS, and MS/MS/MS methods are compared to illustrate trade-offs between sensitivity and selectivity. Filtered Noise Field (FNF) technology is found to be an excellent means for achieving lower detection limits through selective storage of the ion(s) of interest during ionization. Figures of merit including typical sample sizes, detection limits, and response times are provided. The results indicate the potential of these techniques for atmospheric assessments, the High Speed Research Program, and advanced life support monitoring applications for NASA.

  6. An improved linear ion trap physics package

    NASA Technical Reports Server (NTRS)

    Prestage, J. D.

    1993-01-01

    This article describes an improvement in the architecture of the physics package used in the Linear Ion Trap (LIT)-based frequency standard recently developed at JPL. This new design is based on the observation that ions can be moved along the axis of an LIT by applied dc voltages. The state selection and interrogation region can be separated from the more critical microwave resonance region where the multiplied local oscillator signal is compared with the stable atomic transition. This separation relaxes many of the design constraints of the present units. Improvements include increased frequency stability and a substantial reduction in size, mass, and cost of the final frequency standard.

  7. Atomic Clock Based On Linear Ion Trap

    NASA Technical Reports Server (NTRS)

    Prestage, John D.; Dick, G. John

    1992-01-01

    Highly stable atomic clock based on excitation and measurement of hyperfine transition in 199Hg+ ions confined in linear quadrupole trap by radio-frequency and static electric fields. Configuration increases stability of clock by enabling use of enough ions to obtain adequate signal while reducing non-thermal component of motion of ions in trapping field, reducing second-order Doppler shift of hyperfine transition. Features described in NPO-17758 "Linear Ion Trap for Atomic Clock." Frequency standard based on hyperfine transition described in NPO-17456, "Trapped-Mercury-Ion Frequency Standard."

  8. Simple analytic potentials for linear ion traps

    NASA Technical Reports Server (NTRS)

    Janik, G. R.; Prestage, J. D.; Maleki, L.

    1989-01-01

    A simple analytical model was developed for the electric and ponderomotive (trapping) potentials in linear ion traps. This model was used to calculate the required voltage drive to a mercury trap, and the result compares well with experiments. The model gives a detailed picture of the geometric shape of the trapping potenital and allows an accurate calculation of the well depth. The simplicity of the model allowed an investigation of related, more exotic trap designs which may have advantages in light-collection efficiency.

  9. Simple analytic potentials for linear ion traps

    NASA Technical Reports Server (NTRS)

    Janik, G. R.; Prestage, J. D.; Maleki, L.

    1990-01-01

    A simple analytical model was developed for the electric and ponderomotive (trapping) potentials in linear ion traps. This model was used to calculate the required voltage drive to a mercury trap, and the result compares well with experiments. The model gives a detailed picture of the geometric shape of the trapping potential and allows an accurate calculation of the well depth. The simplicity of the model allowed an investigation of related, more exotic trap designs which may have advantages in light-collection efficiency.

  10. New ion trap for frequency standard applications

    NASA Technical Reports Server (NTRS)

    Prestage, J. D.; Dick, G. J.; Maleki, L.

    1989-01-01

    A novel linear ion trap was designed, which permits storage of a large number of ions with reduced susceptibility to the second-order Doppler effect caused by the RF confining fields. This new trap should store about 20 times the number of ions as a conventional RF trap with no corresponding increase in second-order Doppler shift from the confining field. In addition, the sensitivity of this shift to trapping parameters, i.e., RF voltage, RF frequency, and trap size, is greatly reduced.

  11. Cavity QED in a molecular ion trap

    SciTech Connect

    Schuster, D. I.; Bishop, Lev S.; Chuang, I. L.; DeMille, D.; Schoelkopf, R. J.

    2011-01-15

    We propose a class of experiments using rotational states of dipolar molecular ions trapped near an on-chip superconducting microwave cavity. Molecular ions have several advantages over neutral molecules for such cavity quantum electrodynamics experiments. In particular, ions can be loaded easily into deep rf traps and are held independent of their internal state. An analysis of the detection efficiency for, and coherence properties of, the molecular ions is presented. We discuss approaches for manipulating quantum information and performing high-resolution rotational spectroscopy using this system.

  12. Gas amplified ionization detector for gas chromatography

    DOEpatents

    Huston, Gregg C.

    1992-01-01

    A gas-amplified ionization detector for gas chromatrography which possesses increased sensitivity and a very fast response time. Solutes eluding from a gas chromatographic column are ionized by UV photoionization of matter eluting therefrom. The detector is capable of generating easily measured voltage signals by gas amplification/multiplication of electron products resulting from the UV photoionization of at least a portion of each solute passing through the detector.

  13. Tandem-in-space and tandem-in-time mass spectrometry: Triple quadrupoles and quadrupole ion traps

    SciTech Connect

    Johnson, J.V.; Yost, R.A. ); Kelley, P.E.; Bradford, D.C. )

    1990-10-15

    Tandem-in-time and tandem-in-space MS/MS on quadrupole ion trap (ITMS) and triple quadrupole (TQMS) tandem mass spectrometers, respectively, were compared by evaluating the MS/MS daughter spectra, efficiencies of collision-induced dissociation (CID), limits of detection, and dynamic ranges obtained for the methane positive chemical ionization (PCI)-CID of two alkylphosphonates. Although the yield of daughter ions is dependent upon a number of instrumental parameters on both instruments, with judicious selection of parameters the ITMS and TQMS both yielded daughter ions of similar relative abundances. The ITMS had greater efficiencies of fragmentation, collection, and mass selection and transmission of the daughter ions to the detector. With PCI-MS/MS analysis of diisopropyl methylphosphonate standards introduced via capillary gas chromatography, full daughter spectra could be obtained for as little as 15 pg and 1.5 ng injected for the ITMS and the TQMS, respectively.

  14. Ion trap simulation program, ITSIM: A powerful heuristic and predictive tool in ion trap mass spectrometry

    NASA Astrophysics Data System (ADS)

    Bui, Huy Anh

    The multi-particle simulation program, ITSIM version 4.0, takes advantage of the enhanced performance of the Windows 95 and NT operating systems in areas such as memory management, user friendliness, flexibility of graphics and speed, to investigate the motion of ions in the quadrupole ion trap. The objective of this program is to use computer simulations based on mathematical models to improve the performance of the ion trap mass spectrometer. The simulation program can provide assistance in understanding fundamental aspects of ion trap mass spectrometry, precede and help to direct the course of experiments, as well as having didactic value in elucidating and allowing visualization of ion behavior under different experimental conditions. The program uses the improved Euler method to calculate ion trajectories as numerical solutions to the Mathieu differential equation. This Windows version can simultaneously simulate the trajectories of ions with a virtually unlimited number of different mass-to-charge ratios and hence allows realistic mass spectra, ion kinetic energy distributions and other experimentally measurable properties to be simulated. The large number of simulated ions allows examination of (i) the offsetting effects of mutual ion repulsion and collisional cooling in an ion trap and (ii) the effects of higher order fields. Field inhomogeneities arising from exit holes, electrode misalignment, imperfect electrode surfaces or new trap geometries can be simulated with the program. The simulated data are used to obtain mass spectra from mass-selective instability scans as well as by Fourier transformation of image currents induced by coherently moving ion clouds. Complete instruments, from an ion source through the ion trap mass analyzer to a detector, can now be simulated. Applications of the simulation program are presented and discussed. Comparisons are made between the simulations and experimental data. Fourier transformed experiments and a novel six

  15. Extended linear ion trap frequency standard apparatus

    NASA Technical Reports Server (NTRS)

    Prestage, John D. (Inventor)

    1995-01-01

    A linear ion trap for frequency standard applications is provided with a plurality of trapping rods equally spaced and applied quadruple rf voltages for radial confinement of atomic ions and biased level pins at each end for axial confinement of the ions. The trapping rods are divided into two linear ion trap regions by a gap in each rod in a common radial plane to provide dc discontinuity, thus dc isolating one region from the other. A first region for ion-loading and preparation fluorescence is biased with a dc voltage to transport ions into a second region for resonance frequency comparison with a local oscillator derived frequency while the second region is held at zero voltage. The dc bias voltage of the regions is reversed for transporting the ions back into the first region for fluorescence measurement. The dual mode cycle is repeated continuously for comparison and feedback control of the local oscillator derived frequency. Only the second region requires magnetic shielding for the resonance function which is sensitive to any ambient magnetic fields.

  16. ANALYSIS OF POLYCYCLIC AROMATIC HYDROCARBONS BY ION TRAP TANDEM MASS SPECTROMETRY

    EPA Science Inventory

    An ion-trap mass spectrometer with a wave board and tandem mass spectrometry software was used to analyze gas chromatographically separated polycyclic aromatic hydrocarbons (PAHs) by using collision-induced dissociation (CID). The nonresonant (multiple collision) mode was used to...

  17. Temperature programmable microfabricated gas chromatography column

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.

    2003-12-23

    A temperature programmable microfabricated gas chromatography column enables more efficient chemical separation of chemical analytes in a gas mixture by the integration of a resistive heating element and temperature sensing on the microfabricated column. Additionally, means are provided to thermally isolate the heated column from their surroundings. The small heat capacity and thermal isolation of the microfabricated column improves the thermal time response and power consumption, both important factors for portable microanalytical systems.

  18. Soil moisture by extraction and gas chromatography

    NASA Technical Reports Server (NTRS)

    Merek, E. L.; Carle, G. C.

    1973-01-01

    To determine moisture content of soils rapidly and conveniently extract moisture with methanol and determine water content of methanol extract by gas chromatography. Moisture content of sample is calculated from weight of water and methanol in aliquot and weight of methanol added to sample.

  19. APPLICATION OF GAS CHROMATOGRAPHY IN FOOD ANALYSIS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Gas chromatography (GC) is used widely in applications involving food analysis. Typical applications pertain to the quantitative and/or qualitative analysis of food composition, natural products, food additives, flavor and aroma components, a variety of transformation products, and contaminants suc...

  20. Non-planar microfabricated gas chromatography column

    DOEpatents

    Lewis, Patrick R.; Wheeler, David R.

    2007-09-25

    A non-planar microfabricated gas chromatography column comprises a planar substrate having a plurality of through holes, a top lid and a bottom lid bonded to opposite surfaces of the planar substrate, and inlet and outlet ports for injection of a sample gas and elution of separated analytes. A plurality of such planar substrates can be aligned and stacked to provide a longer column length having a small footprint. Furthermore, two or more separate channels can enable multi-channel or multi-dimensional gas chromatography. The through holes preferably have a circular cross section and can be coated with a stationary phase material or packed with a porous packing material. Importantly, uniform stationary phase coatings can be obtained and band broadening can be minimized with the circular channels. A heating or cooling element can be disposed on at least one of the lids to enable temperature programming of the column.

  1. The profiling and identification of the metabolites of 8-prenylkaempferol and a study on their distribution in rats by high-performance liquid chromatography with diode array detection combined with electrospray ionization ion trap time-of-flight multistage mass spectrometry.

    PubMed

    Ma, Li-Man; Xu, Feng; Li, Feng-Chun; Wang, Jing-Zhe; Shang, Ming-Ying; Liu, Guang-Xue; Cai, Shao-Qing

    2016-02-01

    8-Prenylkaempferol is a prenylflavonoid that has various bioactivities and benefits for human health. A high-performance liquid chromatography with a diode array detector combined with electrospray ionization ion trap time-of-flight multistage mass spectrometry (HPLC-DAD-ESI-IT-TOF-MS(n) ) method was established to profile and identify the metabolites of 8-prenylkaempferol in rat in vivo and in vitro, and to study the distribution of these metabolites in rats for the first time. A total of 38 metabolites were detected and tentatively identified, 30 of which were identified as new compounds. The new in vivo metabolic reactions in rats of prenylflavonoids of isomerization, polymerization, sulfation, amino acid conjugation, vitamin C conjugation and other known metabolic reactions were found in the metabolism of 8-prenylkaempferol. The numbers of detected metabolites in feces, urine, plasma, small intestine, stomach, kidneys, liver, heart, lungs, spleen and hepatic S9 fraction were 31, 19, 1, 20, 13, 8, 7, 3, 3, 1 and 11, respectively. This indicated that small intestine and stomach were the major organs in which the 8-prenylkaempferol metabolites were distributed. Furthermore, 16 metabolites were determined to have bioactivities based on the literature and 'PharmMapper' analysis. These findings are useful for better comprehension of the effective forms, target organs and pharmacological actions of 8-prenylkaempferol. Moreover, they provide a reference for the study of the metabolism and distribution of prenylflavonoid aglycone compounds. PMID:26058713

  2. Linear Ion Trap for the Mars Organic Molecule Analyzer

    NASA Astrophysics Data System (ADS)

    Brinckerhoff, William; Arevalo, Ricardo; Danell, Ryan; van Amerom, Friso; Pinnick, Veronica; Li, Xiang; Hovmand, Lars; Getty, Stephanie; Mahaffy, Paul; Goesmann, Fred; Steininger, Harald

    2014-05-01

    The 2018 ExoMars rover mission includes the Mars Organic Molecule Analyzer (MOMA) investigation. MOMA will examine the chemical composition of samples acquired from depths of up to two meters below the martian surface, where organics may be protected from radiative and oxidative degradation. When combined with the complement of instruments in the rover's Pasteur Payload, MOMA has the potential to reveal the presence of a wide range of organics preserved in a variety of mineralogical environments, and to begin to understand the structural character and potential origin of those compounds. MOMA includes a linear, or 2D, ion trap mass spectrometer (ITMS) that is designed to analyze molecular composition of (i) gas evolved from pyrolyzed powder samples and separated on a gas chromatograph and (ii) ions directly desorbed from solid samples at Mars ambient pressure using a pulsed laser and a fast-valve capillary ion inlet system. This "dual source" approach gives MOMA unprecedented breadth of detection over a wide range of molecular weights and volatilities. Analysis of nonvolatile, higher-molecular weight organics such as carboxylic acids and peptides even in the presence of significant perchlorate concentrations is enabled by the extremely short (~1 ns) pulses of the desorption laser. Use of the ion trap's tandem mass spectrometry mode permits selective focus on key species for isolation and controlled fragmentation, providing structural analysis capabilities. The flight-like engineering test unit (ETU) of the ITMS, now under construction, will be used to verify breadboard performance with high fidelity, while simultaneously supporting the development of analytical scripts and spectral libraries using synthetic and natural Mars analog samples guided by current results from MSL. ETU campaign data will strongly advise the specifics of the calibration applied to the MOMA flight model as well as the science operational procedures during the mission.

  3. Characterization of proanthocyanidins from Parkia biglobosa (Jacq.) G. Don. (Fabaceae) by Flow Injection Analysis-Electrospray Ionization Ion Trap Tandem Mass Spectrometry and Liquid Chromatography/Electrospray Ionization Mass Spectrometry.

    PubMed

    Tala, Viviane Raïssa Sipowo; Candida da Silva, Viviane; Rodrigues, Clenilson Martins; Nkengfack, Augustin Ephrem; dos Santos, Lourdes Campaner; Vilegas, Wagner

    2013-01-01

    The present study investigates the chemical composition of the African plant Parkia biglobosa (Fabaceae) roots and barks by Liquid Chromatography-Electrospray Ionization and Direct Injection Tandem Mass Spectrometry analysis. Mass spectral data indicated that B-type oligomers are present, namely procyanidins and prodelphinidins, with their gallate and glucuronide derivatives, some of them in different isomeric forms. The analysis evidenced the presence of up to 40 proanthocyanidins, some of which are reported for the first time. In this study, the antiradical activity of extracts of roots and barks from Parkia biglobosa was evaluated using DPPH method and they showed satisfactory activities. PMID:23455671

  4. Ion traps fabricated in a CMOS foundry

    SciTech Connect

    Mehta, K. K.; Ram, R. J.; Eltony, A. M.; Chuang, I. L.; Bruzewicz, C. D.; Sage, J. M. Chiaverini, J.

    2014-07-28

    We demonstrate trapping in a surface-electrode ion trap fabricated in a 90-nm CMOS (complementary metal-oxide-semiconductor) foundry process utilizing the top metal layer of the process for the trap electrodes. The process includes doped active regions and metal interconnect layers, allowing for co-fabrication of standard CMOS circuitry as well as devices for optical control and measurement. With one of the interconnect layers defining a ground plane between the trap electrode layer and the p-type doped silicon substrate, ion loading is robust and trapping is stable. We measure a motional heating rate comparable to those seen in surface-electrode traps of similar size. This demonstration of scalable quantum computing hardware utilizing a commercial CMOS process opens the door to integration and co-fabrication of electronics and photonics for large-scale quantum processing in trapped-ion arrays.

  5. Ion funnel ion trap and process

    DOEpatents

    Belov, Mikhail E [Richland, WA; Ibrahim, Yehia M [Richland, WA; Clowers, Biran H [West Richland, WA; Prior, David C [Hermiston, OR; Smith, Richard D [Richland, WA

    2011-02-15

    An ion funnel trap is described that includes a inlet portion, a trapping portion, and a outlet portion that couples, in normal operation, with an ion funnel. The ion trap operates efficiently at a pressure of .about.1 Torr and provides for: 1) removal of low mass-to-charge (m/z) ion species, 2) ion accumulation efficiency of up to 80%, 3) charge capacity of .about.10,000,000 elementary charges, 4) ion ejection time of 40 to 200 .mu.s, and 5) optimized variable ion accumulation times. Ion accumulation with low concentration peptide mixtures has shown an increase in analyte signal-to-noise ratios (SNR) of a factor of 30, and a greater than 10-fold improvement in SNR for multiply charged analytes.

  6. Proposed LLNL electron beam ion trap

    SciTech Connect

    Marrs, R.E.; Egan, P.O.; Proctor, I.; Levine, M.A.; Hansen, L.; Kajiyama, Y.; Wolgast, R.

    1985-07-02

    The interaction of energetic electrons with highly charged ions is of great importance to several research fields such as astrophysics, laser fusion and magnetic fusion. In spite of this importance there are almost no measurements of electron interaction cross sections for ions more than a few times ionized. To address this problem an electron beam ion trap (EBIT) is being developed at LLNL. The device is essentially an EBIS except that it is not intended as a source of extracted ions. Instead the (variable energy) electron beam interacting with the confined ions will be used to obtain measurements of ionization cross sections, dielectronic recombination cross sections, radiative recombination cross sections, energy levels and oscillator strengths. Charge-exchange recombinaion cross sections with neutral gasses could also be measured. The goal is to produce and study elements in many different charge states up to He-like xenon and Ne-like uranium. 5 refs., 2 figs.

  7. Flow field thermal gradient gas chromatography.

    PubMed

    Boeker, Peter; Leppert, Jan

    2015-09-01

    Negative temperature gradients along the gas chromatographic separation column can maximize the separation capabilities for gas chromatography by peak focusing and also lead to lower elution temperatures. Unfortunately, so far a smooth thermal gradient over a several meters long separation column could only be realized by costly and complicated manual setups. Here we describe a simple, yet flexible method for the generation of negative thermal gradients using standard and easily exchangeable separation columns. The measurements made with a first prototype reveal promising new properties of the optimized separation process. The negative thermal gradient and the superposition of temperature programming result in a quasi-parallel separation of components each moving simultaneously near their lowered specific equilibrium temperatures through the column. Therefore, this gradient separation process is better suited for thermally labile molecules such as explosives and natural or aroma components. High-temperature GC methods also benefit from reduced elution temperatures. Even for short columns very high peak capacities can be obtained. In addition, the gradient separation is particularly beneficial for very fast separations below 1 min overall retention time. Very fast measurements of explosives prove the benefits of using negative thermal gradients. The new concept can greatly reduce the cycle time of high-resolution gas chromatography and can be integrated into hyphenated or comprehensive gas chromatography setups. PMID:26235451

  8. A new ion mobility-linear ion trap instrument for complex mixture analysis.

    PubMed

    Donohoe, Gregory C; Maleki, Hossein; Arndt, James R; Khakinejad, Mahdiar; Yi, Jinghai; McBride, Carroll; Nurkiewicz, Timothy R; Valentine, Stephen J

    2014-08-19

    A new instrument that couples a low-pressure drift tube with a linear ion trap mass spectrometer is demonstrated for complex mixture analysis. The combination of the low-pressure separation with the ion trapping capabilities provides several benefits for complex mixture analysis. These include high sensitivity, unique ion fragmentation capabilities, and high reproducibility. Even though the gas-phase separation and the mass measurement steps are each conducted in an ion filtering mode, detection limits for mobility-selected peptide ions are in the tens of attomole range. In addition to ion separation, the low-pressure drift tube can be used as an ion fragmentation cell yielding mobility-resolved fragment ions that can be subsequently analyzed by multistage tandem mass spectrometry (MS(n)) methods in the ion trap. Because of the ion trap configuration, these methods can be comprised of any number (limited by ion signal) of collision-induced dissociation (CID) and electron transfer dissociation (ETD) processes. The high reproducibility of the gas-phase separation allows for comparison of two-dimensional ion mobility spectrometry (IMS)-MS data sets in a pixel-by-pixel fashion without the need for data set alignment. These advantages are presented in model analyses representing mixtures encountered in proteomics and metabolomics experiments. PMID:25068446

  9. Neutral fragment filtering for rapid identification of new diester-diterpenoid alkaloids in roots of Aconitum carmichaeli by ultra-high-pressure liquid chromatography coupled with linear ion trap-orbitrap mass spectrometry.

    PubMed

    Zhang, Jing; Huang, Zhi Hai; Qiu, Xiao Hui; Yang, Yi Ming; Zhu, Da Yuan; Xu, Wen

    2012-01-01

    A rapid and effective method was developed for separation and identification of diester-diterpenoid alkaloids (DDA) in the roots of Aconitum carmichaeli by ultra-high-pressure liquid chromatography coupled with high resolution LTQ-Orbitrap tandem mass spectrometry (UHPLC-LTQ-Orbitrap-MS(n)). According to accurate mass measurement and the characteristic neutral loss filtering strategy, a total of 42 diester-diterpenoid alkaloids (DDA) were rapidly detected and characterized or tentatively identified. Meanwhile, the proposed fragmentation pathways and the major diagnostic fragment ions of aconitine, mesaconitine and hypaconitine were investigated to trace DDA derivatives in crude plant extracts. 23 potential new compounds were successfully screened and characterized in Aconitum carmichaeli, including 16 short chain fatty acyls DDA, 4 N-dealkyl DDA and several isomers of aconitine, mesaconitine and hypaconitine. PMID:23285005

  10. Advances in field-portable ion trap GC/MS instrumentation

    NASA Astrophysics Data System (ADS)

    Diken, Eric G.; Arno, Josep; Skvorc, Ed; Manning, David; Andersson, Greger; Judge, Kevin; Fredeen, Ken; Sadowski, Charles; Oliphant, Joseph L.; Lammert, Stephen A.; Jones, Jeffrey L.; Waite, Randall W.; Grant, Chad; Lee, Edgar D.

    2012-06-01

    The rapid and accurate detection and identification of chemical warfare agents and toxic industrial chemicals can be critical to the protection of military and civilian personnel. The use of gas chromatography (GC) - mass spectrometry (MS) can provide both the sensitivity and selectivity required to identify unknown chemicals in complex (i.e. real-world) environments. While most widely used as a laboratory-based technique, recent advances in GC, MS, and sampling technologies have led to the development of a hand-portable GC/MS system that is more practical for field-based analyses. The unique toroidal ion trap mass spectrometer (TMS) used in this instrument has multiple benefits related to size, weight, start-up time, ruggedness, and power consumption. Sample separation is achieved in record time (~ 3 minutes) and with high resolution using a state-of-the-art high-performance low-thermal-mass GC column. In addition to providing a system overview highlighting its most important features, the presentation will focus on the chromatographic and mass spectral performance of the system. Results from exhaustive performance testing of the new instrument will be introduced to validate its unique robustness and ability to identify targeted and unknown chemicals.

  11. Improved Thermal Modulator for Gas Chromatography

    NASA Technical Reports Server (NTRS)

    Hasselbrink, Ernest Frederick, Jr.; Hunt, Patrick J.; Sacks, Richard D.

    2008-01-01

    An improved thermal modulator has been invented for use in a variant of gas chromatography (GC). The variant in question denoted as two-dimensional gas chromatography (2DGC) or GC-GC involves the use of three series-connected chromatographic columns, in the form of capillary tubes coated interiorly with suitable stationary phases (compounds for which different analytes exhibit different degrees of affinity). The two end columns are relatively long and are used as standard GC columns. The thermal modulator includes the middle column, which is relatively short and is not used as a standard GC column: instead, its temperature is modulated to affect timed adsorption and desorption of analyte gases between the two end columns in accordance with a 2DGC protocol.

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

    PubMed

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

    2016-09-10

    An ultra-high performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for simultaneous quantification of six major bioactive compounds in five varieties of Withania somnifera in various plant parts (leaf, stem and root). The analysis was accomplished on Waters ACQUITY UPLC BEH C18 column with linear gradient elution of water/formic acid (0.1%) and acetonitrile at a flow rate of 0.3mLmin(-1). The proposed method was validated with acceptable linearity (r(2), 0.9989-0.9998), precision (RSD, 0.16-2.01%), stability (RSD, 1.04-1.62%) and recovery (RSD ≤2.45%), under optimum conditions. The method was also successfully applied for the simultaneous determination of six marker compounds in twenty-six marketed formulations. Hierarchical cluster analysis and principal component analysis were applied to discriminate these twenty-six batches based on characteristics of the bioactive compounds. The results indicated that this method is advance, rapid, sensitive and suitable to reveal the quality of Withania somnifera and also capable of performing quality evaluation of polyherbal formulations having similar markers/raw herbs. PMID:27475405

  13. Identification of the metabolites after oral administration of extract of ziziphi spinosae semen to rats or dogs by high-performance liquid chromatography/linear ion trap FTICR hybrid mass spectrometry.

    PubMed

    Ren, Yan; Wang, Pengyuan; Wu, Caisheng; Zhang, Jinlan; Niu, Chunyan

    2013-01-01

    Ziziphi spinosae semen (ZSS) is a traditional Chinese medicine that has been widely used to treat insomnia and anxiety. Modern pharmacological studies have demonstrated that flavonoids are the main active compounds in ZSS. However, the metabolites and the metabolic pathways of flavonoids in ZSS have not been investigated thoroughly. In this study, a method based on high-performance liquid chromatography coupled with Fourier transform ion cyclotron resonance mass spectrometry (HPLC/FTICR-MS) was established to identify the metabolites of flavonoids after oral administration of extract of ZSS to rats or dogs, using parent mass list-triggered data-dependent multiple-stage mass analysis at a resolving power of 50,000 in the external calibration mode. The mass accuracies obtained for all full-scan analyses were less than 4 ppm (<2 ppm in most cases). A total of 15 compounds were detected in biological samples of rats and dogs, and nine compounds were identified. The metabolic pathways of flavonoids of ZSS in rats and dogs were proposed. The results may help better understand the material basis and pharmacological mechanism of ZSS. PMID:22522941

  14. Dimethocaine, a synthetic cocaine analogue: studies on its in-vivo metabolism and its detectability in urine by means of a rat model and liquid chromatography-linear ion-trap (high-resolution) mass spectrometry.

    PubMed

    Meyer, Markus R; Lindauer, Carina; Welter, Jessica; Maurer, Hans H

    2014-03-01

    Dimethocaine (DMC, larocaine), a synthetic derivative of cocaine, is a widely distributed "legal high" consumed as a "new psychoactive substance" (NPS) without any safety testing, for example studies of metabolism. Therefore, the purpose of this work was to study its in-vivo and in-vitro metabolism by use of liquid chromatography-(high resolution) mass spectrometry (LC-HRMS(n)). DMC was administered to male Wistar rats (20 mg kg(-1)) and their urine was extracted either by solid-phase extraction after enzymatic cleavage of conjugates or by use of protein precipitation (PP). The metabolites were separated and identified by LC-HRMS(n). The main phase I reactions were ester hydrolysis, deethylation, hydroxylation of the aromatic system, and a combination of these. The main phase II reaction was N-acetylation of the p-aminobenzoic acid part of the unchanged parent compound and of several phase I metabolites. The metabolites identified were then used for identification of DMC in rat urine after application of a common user's dose. By use of GC-MS and LC-MS(n) standard urine-screening approaches (SUSAs), DMC and its metabolites could be detected in the urine samples. PMID:24448968

  15. Proton Transfer Reaction Ion Trap Mass Spectrometer

    SciTech Connect

    Prazeller, Peter; Palmer, Peter T.; Boscaini, Elena; Jobson, B Tom T.; Alexander, M. Lizabeth

    2003-06-11

    Proton transfer reaction mass spectrometry is a relatively new field that has attracted a great deal of interest in the last few years. This technique uses H₃Oþ as a chemical ionization (CI) reagent to measure volatile organic compounds (VOCs) in the parts per billion by volume (ppbv) to parts per trillion by volume (pptv) range. Mass spectra acquired with a proton transfer reaction mass spectrometer (PTR-MS) are simple because proton transfer chemical ionization is ‘soft’ and results in little or no fragmentation. Unfortunately, peak identification can still be difficult due to isobaric interferences. A possible solution to this problem is to couple the PTR drift tube to an ion trap mass spectrometer (ITMS). The use of an ITMS is appealing because of its ability to perform MS/MS and possibly distinguish between isomers and other isobars. Additionally, the ITMS duty cycle is much higher than that of a linear quadrupole so faster data acquisition rates are possible that will allow for detection of multiple compounds. Here we present the first results from a proton transfer reaction ion trap mass spectrometer (PTR-ITMS). The aim of this study was to investigate ion injection and storage efficiency of a simple prototype instrument in order to estimate possible detection limits of a second-generation instrument. Using this prototype a detection limit of 100 ppbv was demonstrated. Modifications are suggested that will enable further reduction in detection limits to the low-ppbv to high-pptv range. Furthermore, the applicability of MS/MS in differentiating between isobaric species was determined. MS/MS spectra of the isobaric compounds methyl vinyl ketone (MVK) and methacrolein (MACR) are presented and show fragments of different mass making differentiation possible, even when a mixture of both species is present in the same sample. However, MS/MS spectra of acetone and propanal produce fragments with the same molecular masses but with different intensity ratios

  16. Proton Transfer Reaction Ion Trap Mass Spectrometer

    SciTech Connect

    Prazeller, Peter; Palmer, Peter T.; Boscaini, Elena; Jobson, B Tom; Alexander, M. Lizabeth

    2003-07-07

    Proton Transfer Reaction Mass Spectrometry (PTR-MS) is a relatively new field that has attracted a great deal of interest in the last several years. This technique uses H3O+ as a chemical ionization (CI) agent for measuring volatile organic compounds (VOCs) in the parts per billion by volume (ppbv) - parts per trillion by volume (pptv) range. PTR-MS mass spectra are simple because the ionization method of proton transfer is “soft”, resulting in little or no fragmentation. Unfortunately, the simplicity of the mass spectra can cause problems in peak identification due to isobaric interferences. A possible solution to this problem is to couple the PTR drift tube to an ion trap mass spectrometer (ITMS). ITMS is appealing because of the ability to perform MS/MS and possibly distinguish between isomers and other isobars. Additionally, the ITMS duty cycle is much higher than that of a linear quadrupole so faster data acquisition rates can be realized for detection of multiple compounds. We present here the first results from a Proton Transfer Reaction Ion Trap Mass Spectrometer (PTR-ITMS). The aim of this study was to investigate ion injection and storage efficiency of a simple prototype interface in order to estimate possible detection limits of a second generation instrument. Using this prototype a detection limit of 100 ppbv was demonstrated for the PTR-ITMS. Modifications are suggested that will enable further reduction in detection limits to the low ppbv to pptv range. Furthermore the applicability of MS/MS to differentiate between isobaric species was determined. MS/MS spectra of the isobaric compounds methyl vinyl ketone (MVK) and methacrolein (MACR) are presented and show fragments of different mass making a differentiation possible even when a mixture of both species is present in the same sample. MS/MS spectra of acetone and propanal produce fragments with the same molecular weight but different ratios, allowing quantitative distinction only if one species

  17. Phase I and II metabolites of speciogynine, a diastereomer of the main Kratom alkaloid mitragynine, identified in rat and human urine by liquid chromatography coupled to low- and high-resolution linear ion trap mass spectrometry.

    PubMed

    Philipp, Anika A; Wissenbach, Dirk K; Weber, Armin A; Zapp, Josef; Maurer, Hans H

    2010-11-01

    Mitragyna speciosa (Kratom in Thai), a Thai medical plant, is misused as herbal drug of abuse. Besides the most abundant alkaloids mitragynine (MG) and paynantheine (PAY), several other alkaloids were isolated from Kratom leaves, among them the third abundant alkaloid is speciogynine (SG), a diastereomer of MG. The aim of this present study was to identify the phase I and II metabolites of SG in rat urine after the administration of a rather high dose of the pure alkaloid and then to confirm these findings using human urine samples after Kratom use. The applied liquid chromatography coupled to low- and high-resolution mass spectrometry (LC-HRMS-MS) provided detailed information on the structure in the MS(n) mode particularly with high resolution. For the analysis of the human samples, the LC separation had to be improved markedly allowing the separation of SG and its metabolites from its diastereomer MG and its metabolites. In analogy to MG, besides SG, nine phase I and eight phase II metabolites could be identified in rat urine, but only three phase I and five phase II metabolites in human urine. These differences may be caused by the lower SG dose applied by the user of Kratom preparations. SG and its metabolites could be differentiated in the human samples from the diastereomeric MG and its metabolites comparing the different retention times determined after application of the single alkaloids to rats. In addition, some differences in MS(2) and/or MS(3) spectra of the corresponding diastereomers were observed. PMID:20967737

  18. Multiresidue trace analysis of sulfonamide antibiotics and their metabolites in soils and sewage sludge by pressurized liquid extraction followed by liquid chromatography-electrospray-quadrupole linear ion trap mass spectrometry.

    PubMed

    García-Galán, María Jesús; Díaz-Cruz, Silvia; Barceló, Damià

    2013-02-01

    The present study describes the development, validation and a practical application of a fully automated analytical method based on pressurized liquid extraction (PLE) followed by solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) for the simultaneous determination of 22 sulfonamides, including five acetylated metabolites, in sewage sludge and soil samples. Both matrix matched calibration curves and standard calibration curves were built in order to evaluate the potential matrix effects during analysis, and different internal standards were used to compensate these effects during quantification. The recovery efficiencies were found to be 60-130% for the majority of the sulfonamides in both matrices and at two spike levels. The intra-day and inter-day precisions, expressed by the relative standard deviation (RSD), were below 23%. The method limits of detection (MLODs) achieved were in the range 0.03-2.23 ng g(-1) for sewage sludge and 0.01-4.19 ng g(-1) for soil samples. The methodology was applied to evaluate the occurrence of the target sulfonamides in several sewage sludge and soil samples taken in different wastewater treatment plants (WWTPs) and agricultural areas. Results confirmed the wide presence of sulfonamides in both matrices, being sulfathiazole and sulfamethazine the sulfonamides most frequently detected in sewage sludge and soil samples, respectively. Maximum concentrations corresponded to sulfamethazine in both cases (139.2 ng g(-1) and 8.53 ng g(-1) for sewage sludge and soils respectively). Levels were generally lower in soils. Three of the five acetylated metabolites were detected in sewage sludge and two of them in soils, at concentrations not higher than 9.81 ng g(-1). PMID:23312557

  19. Monitoring Air Pollution In and Around the Premises of Industrial Parks Using Two Types of Electronic Nose and Gas Chromatography-Ion Trap Mass Spectrometry

    SciTech Connect

    Liu, Jen Yu; Ling, Yong Chien, Sr.

    2004-03-31

    Two types of electronic nose and GC-MS were used to monitor air pollution in the premises of seven industrial parks. Real-time analysis of air at the sites was performed using portable electronic noses. Air samples were analyzed from the up and down stream direction along the wind flow to investigate the effect or distribution of the pollutants on the surrounding environment. The advantage of multisensors in spatially resolved sensing for direct multicomponent analysis was explored to minimize tedious sample preparation procedure. Electronic nose could give characteristic odor fingerprints, which were correlated with the pollutants analyzed using GC-MS providing detailed diagnostic information such as the presence of hydrocarbons, halocarbons, phenols, nitrogenous benzenes, sulfur compounds, lipid-derived compounds, polysiloxanes, etc. Subsequent principal component analysis helped in identifying the source of pollutants. The applicability of the electronic nose was demonstrated confirming it to be a simple and rapid screening method for identifying the pollutant source.

  20. ANALYSIS OF AIRBORNE CARBOXYLIC ACIDS AND PHENOLS AS THEIR PENTAFLUOROBENZYL DERIVATIVES: GAS CHROMATOGRAPHY/ION TRAP MASS SPECTROMETRY WITH A NOVEL CHEMICAL IONIZATION REAGENT, PFBOH. (R826247)

    EPA Science Inventory

    The complex photochemical transformations of biogenic
    hydrocarbons such as isoprene and of anthropogenic
    hydrocarbons such as aromatics are an important source
    of carboxylic acids in the troposphere. The
    identification
    of unknown carboxylic acids can be difficul...

  1. New method to determine free sterols/oxysterols in food matrices using gas chromatography and ion trap mass spectrometry (GC-IT-MS).

    PubMed

    Szterk, Arkadiusz; Pakuła, Lucyna

    2016-05-15

    Sterols/oxysterols in food may be free or bound i.e. esterified with fatty acids. Methods commonly applied to determine those compounds in such matrices (based on various analytical techniques) usually start with hydrolysis of the food lipid fraction, which means that the results are no good indication of concentration of free sterols/oxysterols only. But only free oxysterols are proatherogenic factors, bound ones are not. There are some published methods selectively sensitive to free oxysterols only, but they are capable to determine only a few compounds and feature very low recovery rates. The aim of this work was to develop a method to determine various free (non-esterified) sterols/oxysterols in various food matrices. The developed method is based on the GC-IT-MS technique used in the chemical ionization mode. It was applied to determine 16 different free sterols/oxysterols in egg powder, cheese, butter, milk and salami. Fat extracted from the given matrix is purified on a specially prepared silica-gel bed to separate the sterol fraction from the oxysterol one. Sterols are silylated using N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane BSTFA:TMCS, then GC-IT-MS analysed. The method features high recovery rates (75-95%), high reproducibility (RSD<20%), and sensitivity within the 0.01-0.3 mg 100 g(-1) range, depending on the analysed compound. The method is ideally suited for determination of free sterols/oxysterols. Besides, should total concentration of both free and bound forms be of interest, food lipids may be transesterificated before the silica-gel bed purification step. PMID:26992495

  2. Microwave-assisted solvent extraction and gas chromatography ion trap mass spectrometry procedure for the determination of persistent organochlorine pesticides (POPs) in marine sediment.

    PubMed

    Carro, Nieves; García, Isabel; Ignacio, María; Mouteira, Ana

    2006-07-01

    Microwave-assisted solvent extraction of persistent organochlorine pesticides (POPs) in marine sediment was developed and optimized by means of two-level factorial designs. Six variables (microwave power, extraction time and temperature, amount of sample, solvent volume, and sample moisture) were considered as factors in the optimization process. The results show that the amount of sample to be extracted and solvent volume are statistically significant for the overall recovery of the studied pesticides, although compromise conditions have to be established with the object of avoiding overpressure in closed vessels. After extraction, a clean up step including the use of a silica cartridge was performed prior to chromatographic determination in order to remove interferences. The optimized procedure was compared to conventional Soxhlet extraction. The MS-MS ion preparation mode was applied to improve the sensitivity and selectivity of the chromatographic technique. PMID:16791571

  3. The potential of combining ion trap/MS/MS and TOF/MS for identification of emerging contaminants

    USGS Publications Warehouse

    Ferrer, I.; Furlong, E.T.; Heine, C.E.; Thurman, E.M.

    2002-01-01

    The use of a method combining ion trap tandem mass spectrometry (MS/MS) and time of flight mass spectrometry (TOF/MS) for identification of emerging contaminates was discussed. The two tools together complemented each other in sensitivity, fragmentation and accurate mass determination. Liquid chromatography/electrospray ionization/ion-trap tandem mass spectrometry (LC/ESI/MS/MS), in positive ion mode of operation, was used to separate and identify specific compounds. Diagnostic fragment ions were obtained for a polyethyleneglycol(PEG) homolog by ion trap MS/MS, and fragments were measured by TOF/MS. It was observed that the combined method gave an exact mass measurement that differed from the calculated mass.

  4. Linear ion trap based atomic frequency standard

    NASA Technical Reports Server (NTRS)

    Prestage, John D.; Dick, G. J.; Maleki, Lute

    1991-01-01

    In order to develop a trapped ion-based fieldable frequency standard with stability 1 x 10 to the -13th/sq rt tau for averaging times tau greater than 10,000 s, a hybrid RF/DC linear ion trap was developed which permits storage of large numbers of ions with reduced susceptibility to the second-order Doppler effect caused by the RF confining fields. The authors have confined Hg-199(+) ions in this trap and have measured very high Q transitions with good SNRs. In preliminary measurements they obtained stabilities of 1.6 x 10 to the -13th/sq rt tau (tau between 50 and 800 s) with a 160-mHz wide atomic resonance linewidth and a signal-to-noise ratio of 40 for each measurement cycle. Atomic resonance lines as narrow as 30 mHz on the 40.5-GHz clock transition have been measured with no appreciable reduction in the ion signal. A stability of 7 x 10 to the -14th/sq rt tau is made possible by the signal-to-noise and line Q of this measured transition. Analysis of fundamental sources of frequency instability indicates that a long-term stability of 2 x 10 to the -16th is feasible for this device with existing technology for tau = 10 to the 6th s or more.

  5. Chromatography

    MedlinePlus

    Chromatography is a way of separating two or more chemical compounds. Chemical compounds are chemicals that are ... of chemical compound. There are different kinds of chromatography. These include gas, high pressure liquid, or ion ...

  6. Ultrasensitive characterization of site-specific glycosylation of affinity-purified haptoglobin from lung cancer patient plasma using 10 μm i.d. porous layer open tubular liquid chromatography-linear ion trap collision-induced dissociation/electron transfer dissociation mass spectrometry.

    PubMed

    Wang, Dongdong; Hincapie, Marina; Rejtar, Tomas; Karger, Barry L

    2011-03-15

    Site-specific analysis of protein glycosylation is important for biochemical and clinical research efforts. Glycopeptide analysis using liquid chromatography-collision-induced dissociation/electron transfer dissociation mass spectrometry (LC-CID/ETD-MS) allows simultaneous characterization of the glycan structure and attached peptide site. However, due to the low ionization efficiency of glycopeptides during electrospray ionization, 200-500 fmol of sample per injection is needed for a single LC-MS run, which makes it challenging for the analysis of limited amounts of glycoprotein purified from biological matrixes. To improve the sensitivity of LC-MS analysis for glycopeptides, an ultranarrow porous layer open tubular (PLOT) LC column (2.5 m × 10 μm i.d.) was coupled to a linear ion trap (LTQ) collision-induced dissociation/electron transfer dissociation mass spectrometer to provide sensitive analysis of N-linked protein glycosylation heterogeneity. The potential of the developed method is demonstrated by the characterization of site-specific glycosylation using haptoglobin (Hpt) as a model protein. To limit the amount of haptoglobin to low picomole amounts of protein, we affinity purified it from 1 μL of pooled lung cancer patient plasma. A total of 26 glycoforms/glycan compositions on three Hpt tryptic glycopeptides were identified and quantified from 10 LC-MS runs with a consumption of 100 fmol of Hpt digest (13 ng of protein, 10 fmol per injection). Included in this analysis was the determination of the glycan occupancy level. At this sample consumption level, the high sensitivity of the PLOT LC-LTQ-CID/ETD-MS system allowed glycopeptide identification and structure determination, along with relative quantitation of glycans presented on the same peptide backbone, even for low abundant glycopeptides at the ∼100 amol level. The PLOT LC-MS system is shown to have sufficient sensitivity to allow characterization of site-specific protein glycosylation from trace

  7. Fast and comprehensive multi-residue analysis of a broad range of human and veterinary pharmaceuticals and some of their metabolites in surface and treated waters by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry.

    PubMed

    Gros, Meritxell; Rodríguez-Mozaz, Sara; Barceló, Damià

    2012-07-27

    The present work describes the development of an analytical method, based on automated off-line solid phase extraction (SPE) followed by ultra-high-performance liquid chromatography coupled to quadrupole linear ion trap tandem mass spectrometry (UPLC-QqLIT) for the determination of 81 pharmaceutical residues, covering various therapeutic groups, and some of their main metabolites, in surface and treated waters (influent and effluent wastewaters, river, reservoir, sea and drinking water). For unequivocal identification and confirmation, two selected reaction monitoring (SRM) transitions per compound are monitored. Quantification is performed by the internal standard approach, indispensable to correct matrix effects. Moreover, to obtain an extra tool for confirmation of positive findings, an information dependent acquisition (IDA) experiment was performed, with SRM as survey scan and an enhanced product ion (EPI) scan as dependent scan. Compound identification was carried out by library search, matching the EPI spectra achieved at one fixed collision energy with those present in a library. The main advantages of the method are automation and speed-up of sample preparation by the reduction of extraction volumes for some matrices, the fast separation of a big number of pharmaceuticals, its high sensitivity (limits of detection in the low ng/L range), selectivity, due to the use of tandem mass spectrometry, reliability since a significant number of isotopically labeled compounds are used as internal standards for quantification and finally, the analysis of tap, reservoir and sea waters, since information about occurrence of pharmaceuticals in these matrices is still sparse. As part of the validation procedure, the method developed was applied to the analysis of pharmaceutical residues in waste and surface waters from different sites in Catalonia (North East of Spain). PMID:22704668

  8. HDT mixtures treatment strategies by gas chromatography

    SciTech Connect

    Laquerbe, C.; Contreras, S.; Demoment, J.

    2008-07-15

    Gas phase chromatographic processes are of interest for the separation of hydrogen isotopes from an HDT mixture. For a certain quantity, they are very competitive and present several benefits. Nevertheless no active packing material allows to have simultaneously good enrichment performances for tritium production and high decontamination capabilities for HD gases. The influence of the packing material is first described in this article. Then two specific processes (TCAP and Reverse Chromatography), each well adapted to perform one target, are presented. Finally, the problematic to propose an optimized treatment scheme associating these two processes is formulated. (authors)

  9. Four-Sector Cylindrical Radio-Frequency Ion Trap

    NASA Technical Reports Server (NTRS)

    Melbourne, Ruthann K.; Prestage, John D.; Maleki, Lutfollah

    1992-01-01

    Proposed linear radio-frequency ion trap consists of closed metal cylinder partitioned into four equal cylindrical-sector electrodes and two circular end electrodes. Features include relatively large ion-storage capacity and shielding against external fields. Used in frequency-standard laboratories to confine 199Hg+ ions electrodynamically in isolation from external environment. Similar to device described in "Linear Ion Trap for Atomic Clock" (NPO-17758).

  10. Three-Dimensional Array for 40Ca+ Ion Trapping

    NASA Astrophysics Data System (ADS)

    Wan, Jin-Yin; Liu, Liang

    2009-04-01

    We present a three-dimensional scalable linear ion trap scheme for ion trapping and discuss its applications for the optical frequency standard and scalable quantum information processing with its parallel strings of trapped 40Ca+ ions. The geometry here contains nine equal-distance parallel rods driven by rf, which form trapping potentials for radial confinement and two end ring electrodes biased at a few volts for axial confinement. Its feasibility is calculated by using the finite element analysis method.

  11. Design and operation of the electron beam ion trap

    SciTech Connect

    Vogel, D.

    1990-05-30

    This report describes the basic features and operating principles of the Electron Beam Ion Trap. The differences between EBIT and other sources of highly charged ions are outlined. Its features and operating parameters are discussed. The report also explains why certain design choices were necessary and the constraints involved in building an electron beam ion trap. EBIT's evaporation cooling system is described in detail. 13 refs., 8 figs.

  12. Permanent gas analysis using gas chromatography with vacuum ultraviolet detection.

    PubMed

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Fan, Hui; Hildenbrand, Zacariah; Wong, Derek; Wetz, David; Schug, Kevin A

    2015-04-01

    The analysis of complex mixtures of permanent gases consisting of low molecular weight hydrocarbons, inert gases, and toxic species plays an increasingly important role in today's economy. A new gas chromatography detector based on vacuum ultraviolet (VUV) spectroscopy (GC-VUV), which simultaneously collects full scan (115-240 nm) VUV and UV absorption of eluting analytes, was applied to analyze mixtures of permanent gases. Sample mixtures ranged from off-gassing of decomposing Li-ion and Li-metal batteries to natural gas samples and water samples taken from private wells in close proximity to unconventional natural gas extraction. Gas chromatography separations were performed with a porous layer open tubular column. Components such as C1-C5 linear and branched hydrocarbons, water, oxygen, and nitrogen were separated and detected in natural gas and the headspace of natural gas-contaminated water samples. Of interest for the transport of lithium batteries were the detection of flammable and toxic gases, such as methane, ethylene, chloromethane, dimethyl ether, 1,3-butadiene, CS2, and methylproprionate, among others. Featured is the capability for deconvolution of co-eluting signals from different analytes. PMID:25724098

  13. Axial thermal gradients in microchip gas chromatography.

    PubMed

    Wang, Anzi; Hynynen, Sampo; Hawkins, Aaron R; Tolley, Samuel E; Tolley, H Dennis; Lee, Milton L

    2014-12-29

    Fabrication technologies for microelectromechanical systems (MEMS) allow miniaturization of conventional benchtop gas chromatography (GC) to portable, palm-sized microfabricated GC (μGC) devices, which are suitable for on-site chemical analysis and remote sensing. The separation performance of μGC systems, however, has not been on par with conventional GC. Column efficiency, peak symmetry and resolution are often compromised by column defects and non-ideal injections. The relatively low performance of μGC devices has impeded their further commercialization and broader application. In this work, the separation performance of μGC columns was improved by incorporating thermal gradient gas chromatography (TGGC). The analysis time was ∼20% shorter for TGGC separations compared to conventional temperature-programmed GC (TPGC) when a wide sample band was introduced into the column. Up to 50% reduction in peak tailing was observed for polar analytes, which improved their resolution. The signal-to-noise ratios (S/N) of late-eluting peaks were increased by 3-4 fold. The unique focusing effect of TGGC overcomes many of the previous shortcomings inherent in μGC analyses. PMID:25476685

  14. Cryogenic Linear Ion Trap for Large-Scale Quantum Simulations

    NASA Astrophysics Data System (ADS)

    Pagano, Guido; Hess, Paul; Kaplan, Harvey; Birckelbaw, Eric; Hernanez, Micah; Lee, Aaron; Smith, Jake; Zhang, Jiehang; Monroe, Christopher

    2016-05-01

    Ions confined in RF Paul traps are a useful tool for quantum simulation of long-range spin-spin interaction models. As the system size increases, classical simulation methods become incapable of modeling the exponentially growing Hilbert space, necessitating quantum simulation for precise predictions. Current experiments are limited to less than 30 qubits due to collisions with background gas that regularly destroys the ion crystal. We present progress toward the construction of a cryogenic ion trap apparatus, which uses differential cryopumping to reduce vacuum pressure to a level where collisions do not occur. This should allow robust trapping of about 100 ions/qubits in a single chain with long lifetimes. Such a long chain will provide a platform to investigate simultaneously cooling of various vibrational modes and will enable quantum simulations that outperform their classical counterpart. Our apparatus will provide a powerful test-bed to investigate a large variety of Hamiltonians, including spin 1 and spin 1/2 systems with Ising or XY interactions. This work is supported by the ARO Atomic Physics Program, the AFOSR MURI on Quantum Measurement and Verification, the IC Fellowship Program and the NSF Physics Frontier Center at JQI.

  15. Cryogenic Linear Ion Trap for Large-Scale Quantum Simulations

    NASA Astrophysics Data System (ADS)

    Kaplan, H. B.; Hess, P. W.; Pagano, G.; Birckelbaw, E. J.; Hernandez, M.; Lee, A. C.; Smith, J.; Zhang, J.; Monroe, C.

    2016-05-01

    Ions confined in RF Paul traps are a useful tool for quantum simulation of long-range spin-spin interaction models. As the system size increases, classical simulation methods become incapable of modeling the exponentially growing Hilbert space, necessitating quantum simulation for precise predictions. Current experiments are limited to less than 30 qubits due to collisions with background gas that regularly destroys the ion crystal. We present progress toward the construction of a cryogenic ion trap apparatus, which uses differential cryopumping to reduce vacuum pressure to a level where collisions do not occur. This should allow robust trapping of about 100 ions/qubits in a single chain with long lifetimes. Such a long chain will provide a platform to investigate simultaneously cooling of various vibrational modes and will enable quantum simulations that outperform their classical counterpart. Our apparatus will provide a powerful test-bed to investigate a large variety of Hamiltonians, including spin 1 and spin 1/2 systems with Ising or XY interactions. This work is supported by the ARO Atomic Physics Program, the AFOSR MURI on Quantum Measurement and Verification, and the NSF Physics Frontier Center at JQI.

  16. Vibrational Cooling in A Cold Ion Trap: Vibrationally Resolved Photoelectron Spectroscopy of Cold C60- Anions

    SciTech Connect

    Wang, Xue B.; Woo, Hin-koon; Wang, Lai S.

    2005-08-01

    We demonstrate vibrational cooling of anions via collisions with a background gas in an ion trap attached to a cryogenically controlled cold head (10 ? 400 K). Photoelectron spectra of vibrationally cold C60- anions, produced by electrospray ionization and cooled in the cold ion trap, have been obtained. Relative to spectra taken at room temperature, vibrational hot bands are completely eliminated, yielding well resolved vibrational structures and a more accurate electron affinity for neutral C60. The electron affinity of C60 is measured to be 2.683 ? 0.008 eV. The cold spectra reveal complicated vibrational structures for the transition to the C60 ground state due to the Jahn-Teller effect in the ground state of C60-. Vibrational excitations in the two Ag modes and eight Hg modes are observed, providing ideal data to assess the vibronic couplings in C60-.

  17. Frequency-scanning MALDI linear ion trap mass spectrometer for large biomolecular ion detection.

    PubMed

    Lu, I-Chung; Lin, Jung Lee; Lai, Szu-Hsueh; Chen, Chung-Hsuan

    2011-11-01

    This study presents the first report on the development of a matrix-assisted laser desorption ionization (MALDI) linear ion trap mass spectrometer for large biomolecular ion detection by frequency scan. We designed, installed, and tested this radio frequency (RF) scan linear ion trap mass spectrometer and its associated electronics to dramatically extend the mass region to be detected. The RF circuit can be adjusted from 300 to 10 kHz with a set of operation amplifiers. To trap the ions produced by MALDI, a high pressure of helium buffer gas was employed to quench extra kinetic energy of the heavy ions produced by MALDI. The successful detection of the singly charged secretory immunoglobulin A ions indicates that the detectable mass-to-charge ratio (m/z) of this system can reach ~385 000 or beyond. PMID:21932813

  18. Ion trap array mass analyzer: structure and performance.

    PubMed

    Li, Xiaoxu; Jiang, Gongyu; Luo, Chan; Xu, Fuxing; Wang, Yuanyuan; Ding, Li; Ding, Chuan-Fan

    2009-06-15

    An ion trap array (ITA) mass analyzer--a novel ion trap mass analyzer with multiple ion trapping and analyzing channels--was designed and constructed. Its property and performance were investigated and reported in this paper. The ITA was built with several planar electrodes including two parallel printed circuit board (PCB) plates. Each PCB plate was fabricated to several identical rectangular electric strips based on normal PCB fabrication technology and was placed symmetrically to those on the opposite plate. There is no electrode between any two adjacent strips. Every strip was supplied with an rf voltage while the polarity of the voltage applied to the adjacent two strips was opposite. So the electric potential at the central plane between two adjacent strips is zero. Multiple identical electric field regions that contain the dominant quadrupole plus some other high-order fields were produced between the two PCB plates. The multiple identical electric field regions will have the property of ion trapping, ion storage, and mass analysis functions. So an ITA could work as multiple ion trap mass analyzers. It could perform multiple sample ion storage, mass-selected ion isolation, ion ejection, and mass analysis simultaneously. The ITA was operated at both "digital ion trap mode" and "conventional rf mode" experimentally. A preliminary mass spectrum has been carried out in one of the ion trap channels, and it shows a mass resolution of over 1000. Additional functions such as mass-selected ion isolation and mass-selected ion ejection have also been tested. Furthermore, the ITA has a small size and very low cost. An ITA with four channels is less than 30 cm(3) in total volume, and it shows a great promise for the miniaturization of the whole mass spectrometer instrument and high-throughput mass analysis. PMID:19441854

  19. An Inexpensive Detector for Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Smith, Allan L.; Thorne, Edward J.; Nadler, Wolfgang

    1998-09-01

    We have developed a low-cost (parts cost approximately $70) detector that can be used in a freshman level class to demonstrate the fundamental principles of gas chromatography (GC). The detector box can be used in a modification of experiments available in the literature which do not enable a quantitative method of analysis. We have used it with success in a freshman class of approximately 450 students in an experiment to separate chlorinated hydrocarbons via GC. Natural gas is used as the carrier gas, a commercial GC column packing is the separating medium, and a Beilstein detector generates a green flame when the halocarbon is burned as it exits the column. The detector box is equipped with a CdS detector selective for the green light emitted and gives a signal that is quantitatively measured by an appropriate means such as a strip chart recorder or computer interfaced terminal panel. The detector box has a limit of detection on the order of 0.5 to 5 mg and shows a linear response over a sixfold change in concentration. Very small volumes (only about 0.1 ml) of most halocarbon vapors are necessary to achieve a measurable signal.

  20. Atomic ion clock with two ion traps, and method to transfer ions

    NASA Technical Reports Server (NTRS)

    Prestage, John D. (Inventor); Chung, Sang K. (Inventor)

    2011-01-01

    An atomic ion clock with a first ion trap and a second ion trap, where the second ion trap is of higher order than the first ion trap. In one embodiment, ions may be shuttled back and forth from one ion trap to the other by application of voltage ramps to the electrodes in the ion traps, where microwave interrogation takes place when the ions are in the second ion trap, and fluorescence is induced and measured when the ions are in the first ion trap. In one embodiment, the RF voltages applied to the second ion trap to contain the ions are at a higher frequency than that applied to the first ion trap. Other embodiments are described and claimed.

  1. Analysis assessment expert system for gas chromatography

    SciTech Connect

    Elling, J.W.; Roberts, R.S.; Lahiri, S.

    1995-12-01

    An artificial intelligence based analysis assessment system is presented to automate gas chromatography instrument troubleshooting. This system is capable of recognizing symptoms of common problems with GC analysis, reasoning with the symptoms to make a problem diagnosis, and suggest appropriate solutions. In this system, signal processing techniques are used to search for symptoms of problems in the time-series data. For example, peak shapes are analyzed for fronting and tailing and the baseline is analyzed for drift and the presence of electronic spikes. A measurement of the severity of each symptom is then used by the expert system to diagnose potential problems with the analysis. This system will be integrated with the instrument control and laboratory automation that is necessary to effect the recommended solutions when possible. The result will be a more robust instrument capable of recognizing failures and error modes from the sample data and capable of correcting many of the common failures.

  2. Kinetic plots for programmed temperature gas chromatography.

    PubMed

    Jespers, Sander; Roeleveld, Kevin; Lynen, Frederic; Broeckhoven, Ken; Desmet, Gert

    2016-06-10

    The applicability of the kinetic plot theory to temperature-programmed gas chromatography (GC) has been confirmed experimentally by measuring the efficiency of a temperature gradient separation of a simple test mixture on 15, 30, 60 and 120m long (coupled) columns. It has been shown that the temperature-dependent data needed for the kinetic plot calculation can be obtained from isothermal experiments at the significant temperature, a temperature that characterizes the entire gradient run. Furthermore, optimal flow rates have been calculated for various combinations of column length, diameter, and operating temperature (or significant temperature). The tabulated outcome of these calculations provide good starting points for the optimization of any GC separation. PMID:27179678

  3. Freeze drying for gas chromatography stationary phase deposition

    DOEpatents

    Sylwester, Alan P.

    2007-01-02

    The present disclosure relates to methods for deposition of gas chromatography (GC) stationary phases into chromatography columns, for example gas chromatography columns. A chromatographic medium is dissolved or suspended in a solvent to form a composition. The composition may be inserted into a chromatographic column. Alternatively, portions of the chromatographic column may be exposed or filled with the composition. The composition is permitted to solidify, and at least a portion of the solvent is removed by vacuum sublimation.

  4. Identification of 11-Nor-delta9-tetrahydrocannabinol-9-carboxylic acid in urine by ion trap GC-MS-MS in the context of doping analysis.

    PubMed

    Caballero, Gerardo M; D'Angelo, Carlos; Fraguío, Mariá Sol; Centurión, Osvaldo Teme

    2004-01-01

    The purpose of this study is to develop a sensitive and specific alternative to current gas chromatography (GC)-mass spectrometry (MS) selected ion monitoring confirmation methods of 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid (cTHC) in human urine samples, in the context of doping analysis. An identification procedure based on the comparison, among suspicious and control samples, of the relative abundances of cTHC selected product ions obtained by GC-tandem MS in an ion trap is presented. The method complies with the identification criteria for qualitative assays established by sports authorities; the comparison procedure is precise, reproducible, specific, and sensitive, thus indicating that it is fit for the purpose of identification accordingly to World Antidoping Agency requirements. PMID:15768841

  5. Applications of resistive heating in gas chromatography: a review.

    PubMed

    Jacobs, Matthew R; Hilder, Emily F; Shellie, Robert A

    2013-11-25

    Gas chromatography is widely applied to separate, identify, and quantify components of samples in a timely manner. Increasing demand for analytical throughput, instrument portability, environmental sustainability, and more economical analysis necessitates the development of new gas chromatography instrumentation. The applications of resistive column heating technologies have been espoused for nearly thirty years and resistively heated gas chromatography has been commercially available for the last ten years. Despite this lengthy period of existence, resistively heated gas chromatography has not been universally adopted. This low rate of adoption may be partially ascribed to the saturation of the market with older convection oven technology, coupled with other analytical challenges such as sampling, injection, detection and data processing occupying research. This article assesses the advantages and applications of resistive heating in gas chromatography and discusses practical considerations associated with adoption of this technology. PMID:24216193

  6. Vacuum ultraviolet detector for gas chromatography.

    PubMed

    Schug, Kevin A; Sawicki, Ian; Carlton, Doug D; Fan, Hui; McNair, Harold M; Nimmo, John P; Kroll, Peter; Smuts, Jonathan; Walsh, Phillip; Harrison, Dale

    2014-08-19

    Analytical performance characteristics of a new vacuum ultraviolet (VUV) detector for gas chromatography (GC) are reported. GC-VUV was applied to hydrocarbons, fixed gases, polyaromatic hydrocarbons, fatty acids, pesticides, drugs, and estrogens. Applications were chosen to feature the sensitivity and universal detection capabilities of the VUV detector, especially for cases where mass spectrometry performance has been limited. Virtually all chemical species absorb and have unique gas phase absorption cross sections in the approximately 120-240 nm wavelength range monitored. Spectra are presented, along with the ability to use software for deconvolution of overlapping signals. Some comparisons with experimental synchrotron data and computed theoretical spectra show good agreement, although more work is needed on appropriate computational methods to match the simultaneous broadband electronic and vibronic excitation initiated by the deuterium lamp. Quantitative analysis is governed by Beer-Lambert Law relationships. Mass on-column detection limits reported for representatives of different classes of analytes ranged from 15 (benzene) to 246 pg (water). Linear range measured at peak absorption for benzene was 3-4 orders of magnitude. Importantly, where absorption cross sections are known for analytes, the VUV detector is capable of absolute determination (without calibration) of the number of molecules present in the flow cell in the absence of chemical interferences. This study sets the stage for application of GC-VUV technology across a wide breadth of research areas. PMID:25079505

  7. Electron source for a mini ion trap mass spectrometer

    DOEpatents

    Dietrich, Daniel D.; Keville, Robert F.

    1995-01-01

    An ion trap which operates in the regime between research ion traps which can detect ions with a mass resolution of better than 1:10.sup.9 and commercial mass spectrometers requiring 10.sup.4 ions with resolutions of a few hundred. The power consumption is kept to a minimum by the use of permanent magnets and a novel electron gun design. By Fourier analyzing the ion cyclotron resonance signals induced in the trap electrodes, a complete mass spectra in a single combined structure can be detected. An attribute of the ion trap mass spectrometer is that overall system size is drastically reduced due to combining a unique electron source and mass analyzer/detector in a single device. This enables portable low power mass spectrometers for the detection of environmental pollutants or illicit substances, as well as sensors for on board diagnostics to monitor engine performance or for active feedback in any process involving exhausting waste products.

  8. Electron source for a mini ion trap mass spectrometer

    DOEpatents

    Dietrich, D.D.; Keville, R.F.

    1995-12-19

    An ion trap is described which operates in the regime between research ion traps which can detect ions with a mass resolution of better than 1:10{sup 9} and commercial mass spectrometers requiring 10{sup 4} ions with resolutions of a few hundred. The power consumption is kept to a minimum by the use of permanent magnets and a novel electron gun design. By Fourier analyzing the ion cyclotron resonance signals induced in the trap electrodes, a complete mass spectra in a single combined structure can be detected. An attribute of the ion trap mass spectrometer is that overall system size is drastically reduced due to combining a unique electron source and mass analyzer/detector in a single device. This enables portable low power mass spectrometers for the detection of environmental pollutants or illicit substances, as well as sensors for on board diagnostics to monitor engine performance or for active feedback in any process involving exhausting waste products. 10 figs.

  9. Computer Modeling of an Ion Trap Mass Analyzer, Part I: Low Pressure Regime

    NASA Astrophysics Data System (ADS)

    Nikolić, Dragan; Madzunkov, Stojan M.; Darrach, Murray R.

    2015-12-01

    We present the multi-particle simulation program suite Computational Ion Trap Analyzer (CITA) designed to calculate the ion trajectories within a Paul quadrupole ion trap developed by the Jet Propulsion Laboratory (JPL). CITA uses an analytical expression of the electrodynamic field, employing up to six terms in multipole expansion and a modified velocity-Verlet method to numerically calculate ion trajectories. The computer code is multithreaded and designed to run on shared-memory architectures. CITA yields near real-time simulations with full propagation of 26 particles per second per core. As a consequence, a realistic numbers of trapped ions (100+ million) can be used and their trajectories modeled, yielding a representative prediction of mass spectrometer analysis of trace gas species. When the model is compared with experimental results conducted at low pressures using the conventional quadrupole and dipole excitation modes, there is an excellent agreement with the observed peak shapes. Owing to the program's efficiency, CITA has been used to explore regions of trapping stability that are of interest to experimental research. These results are expected to facilitate a fast and reliable modeling of ion dynamics in miniature quadrupole ion trap and improve the interpretation of observed mass spectra.

  10. Computer Modeling of an Ion Trap Mass Analyzer, Part I: Low Pressure Regime.

    PubMed

    Nikolić, Dragan; Madzunkov, Stojan M; Darrach, Murray R

    2015-12-01

    We present the multi-particle simulation program suite Computational Ion Trap Analyzer (CITA) designed to calculate the ion trajectories within a Paul quadrupole ion trap developed by the Jet Propulsion Laboratory (JPL). CITA uses an analytical expression of the electrodynamic field, employing up to six terms in multipole expansion and a modified velocity-Verlet method to numerically calculate ion trajectories. The computer code is multithreaded and designed to run on shared-memory architectures. CITA yields near real-time simulations with full propagation of 26 particles per second per core. As a consequence, a realistic numbers of trapped ions (100+ million) can be used and their trajectories modeled, yielding a representative prediction of mass spectrometer analysis of trace gas species. When the model is compared with experimental results conducted at low pressures using the conventional quadrupole and dipole excitation modes, there is an excellent agreement with the observed peak shapes. Owing to the program's efficiency, CITA has been used to explore regions of trapping stability that are of interest to experimental research. These results are expected to facilitate a fast and reliable modeling of ion dynamics in miniature quadrupole ion trap and improve the interpretation of observed mass spectra. Graphical Abstract ᅟ. PMID:26286456

  11. Direct sampling ion trap mass spectrometry vs. GC/MS for monitoring VOCs in groundwater

    SciTech Connect

    Wise, M.B.; Merriweather, R.; Guerin, M.R.

    1995-12-31

    Direct Sampling Ion Trap Mass Spectrometry (DSITMS) has been under refinement and demonstration by this laboratory for several years. The general technology is applicable to a wide range of problems which would benefit from high sample throughput, fast availability of results, and relatively low cost per sample analysis when compared with conventional analytical methods. At the present time, DSITMS can be used to determine targeted analytes in air, water, soil, and other media. This is accomplished by equipping an ion trap with a direct inlet system which consists of a splitter, capillary restrictor, and a set of sample inlet modules. The capillary restrictor provides the interface between atmosphere and the vacuum in the ion trap while the splitter enables sampling modules which require high gas flow rates to be used with the system. The sampling modules consist of a purge module for analyzing VOCs in water or soil, a direct air sampling module, and a thermal desorber. These modules are designed to be easily interchanged by means of quick connect fittings and a single electrical cable. In general, the DSITMS sample inlet system works equally well on all of the commercially available ion traps with which it has been tested including the Finnigan MAT ITMS, Finnigan MAT Magnum, Varian Saturn, and the Teledyne 3D-Q. Both the Magnum and 3D-Q instruments have been utilized for field applications as well as laboratory analysis. This particular study is a comparison of DSITMS with a purge and trap GC/MS for compliance monitoring of VOC`s in groundwater.

  12. Dual-Ion-Trap Frequency Standards With Overlapping Cycles

    NASA Technical Reports Server (NTRS)

    Dick, G. John; Prestage, John D.

    1992-01-01

    Proposed scheme for enhancing performances of atomic frequency-standard apparatuses calls for two or more ion traps per apparatus interrogated in alternation by radio-frequency pulses. Provides nearly constant feedback gain, thereby providing nearly constant corrections for fluctuations in frequency of local oscillator. Degradation of performance by fluctuations in local oscillators reduced.

  13. Quantum Communication in the Ion-Trapped System

    NASA Astrophysics Data System (ADS)

    Xu, Xiong

    2016-03-01

    A theoretical scheme of quantum communication is proposed in the context of ion-trapped systems. According to the results, the receiver can obtain different secret messages in a deterministic way. Our scheme is insensitive to both the initial vibrational state and heating. The probability of the success in our scheme is 1.0.

  14. Optical cavity integrated surface ion trap for enhanced light collection

    NASA Astrophysics Data System (ADS)

    Benito, Francisco M.

    Ion trap systems allow the faithful storage and manipulation of qubits encoded in the energy levels of the ions, and can be interfaced with photonic qubits that can be transmitted to connect remote quantum systems. Single photons transmitted from two remote sites, each entangled with one quantum memory, can be used to entangle distant quantum memories by interfering on a beam splitter. Efficient remote entanglement generation relies upon efficient light collection from single ions into a single mode fiber. This can be realized by integrating an ion trap with an optical cavity and employing the Purcell effect for enhancing the light collection. Remote entanglement can be used as a resource for a quantum repeater for provably secure long-distance communication or as a method for communicating within a distributed quantum information processor. We present the integration of a 1 mm optical cavity with a micro-fabricated surface ion trap. The plano-concave cavity is oriented normal to the chip surface where the planar mirror is attached underneath the trap chip. The cavity is locked using a 780 nm laser which is stabilized to Rubidium and shifted to match the 369 nm Doppler transition in Ytterbium. The linear ion trap allows ions to be shuttled in and out of the cavity mode. The Purcell enhancement of spontaneous emission into the cavity mode would then allow efficient collection of the emitted photons, enabling faster remote entanglement generation.

  15. Differentially pumped dual linear quadrupole ion trap mass spectrometer

    SciTech Connect

    Owen, Benjamin C.; Kenttamaa, Hilkka I.

    2015-10-20

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

  16. Spectroscopy of ions using fast beams and ion traps

    SciTech Connect

    Pinnington, E H; Trabert, E

    2004-10-01

    A knowledge of the spectra of ionized atoms is of importance in many fields. They can be studied in a wide variety of light sources. In recent years techniques coming under the broad heatings of fast beams and ion traps have been used extensively for such investigations. This article considers the advantages that various techniques have for particular applications.

  17. Mixed Stationary Liquid Phases for Gas-Liquid Chromatography.

    ERIC Educational Resources Information Center

    Koury, Albert M.; Parcher, Jon F.

    1979-01-01

    Describes a laboratory technique for use in an undergraduate instrumental analysis course that, using the interpretation of window diagrams, prepares a mixed liquid phase column for gas-liquid chromatography. A detailed procedure is provided. (BT)

  18. ENVIRONMENTAL APPLICATION OF GAS CHROMATOGRAPHY/ATOMIC EMISSION DETECTION

    EPA Science Inventory

    A gas chromatography/atomic emission detector (GC/AED) system has been evaluated for its applicability to environmental analysis. Detection limits, elemental response factors, and regression analysis data were determined for 58 semivolatile environmental contaminants. Detection l...

  19. PRACTICAL FAST GAS CHROMATOGRAPHY FOR CONTRACT LABORATORY PROGRAM PESTICIDE ANALYSES

    EPA Science Inventory

    An approach to shortening the analysis time for practical fast gas chromatography (GC) by using Method Translator software, which can be downloaded free from the Internet, is presented. This sofware simplifies the process of optimizing temperature programming while changing colu...

  20. Solid surface mapping by inverse gas chromatography.

    PubMed

    Gutiérrez, M C; Osuna, S; Baráibar, I

    2005-09-16

    Inverse gas chromatography (IGC) at infinite dilution, is a technique for characterising solid surfaces. Current practice is the injection of n-alkane homologous series to obtain the free energy of adsorption of the CH2 group, from which the London component of the solid surface free energy, gamma(d)s, is calculated. A value around 40 mJ/m2 is obtained for poly(ethylene), and 30 mJ/m2 for a clean glass fibre, while the potential surface interactivity of a glass fibre is far greater than that of poly(ethylene). A specific component of the surface, in mJ/m2, should be calculated in order to obtain significant parameters. As applied up to date, when calculating the specific component of the surface energy, the fact that W(sp)a energy values are in a totally different scale than AN or DN values is a major drawback. Consequently, Ka and Kb values obtained are in arbitrary energy units, different from those of the London component measured by injecting the n-alkane series. This paper proposes a method to obtain Ka and Kb values of the surface in the same energetic scale than the London component. The method enables us to correct the traditional London component of a solid, obtaining a new value, where the amount of WaCH2 accounting for Debye interactions with polar sites, is excluded. As a result, an approach to surface mapping is performed in several different substrate materials. We show results obtained on different solid surfaces: poly(ethylene), clean glass fibre, glass beads, chemically modified glass beads and carbon fibre. PMID:16130707

  1. How far can ion trap miniaturization go? Parameter scaling and space-charge limits for very small cylindrical ion traps.

    PubMed

    Tian, Yuan; Higgs, Jessica; Li, Ailin; Barney, Brandon; Austin, Daniel E

    2014-03-01

    A broad effort is underway to make radiofrequency (RF) ion trap mass spectrometers small enough for portable chemical analysis. A variety of trap geometries and fabrication approaches are under development from several research groups. A common issue is the reduced trapping capacity in smaller traps, with the associated reduction in sensitivity. This article explores the key variables that scale with trap size including RF voltage, frequency, electrical capacitance, power and pseudopotential well depth. High-field electric breakdown constrains the maximum RF voltages used in smaller ion traps. Simulations show the effects of space charge and the limits of trapping capacity as a function of trap dimensions for cylindrical ion traps down to the micrometer level. RF amplitudes that scale as the 1/3, 1/2 and 2/3 power of trap radius, r0, were studied. At a fixed level of performance, the number of analyzable ions scales as r0(n), with n ranging from 1.55 to 1.75 depending on the choice of voltage scaling. The implications for miniaturized ion trap mass spectrometry are discussed. PMID:24619549

  2. Enantioselective gas chromatography/mass spectrometry of methylsulfonyl PCBs with application to arctic marine mammals.

    PubMed

    Wiberg, K; Letcher, R; Sandau, C; Duffe, J; Norstrom, R; Haglund, P; Bidleman, T

    1998-09-15

    Four different commercially available cyclodextrin (CD) capillary gas chromatography (GC) columns were tested for the enantioselective separation of nine environmentally persistent atropisomeric 3- and 4-methylsulfonyl PCBs (MeSO2-CBs). The selected columns contained cyclodextrins with various cavity diameters (beta- or gamma-CD), which were methylated and/or tert-butyldimethylsilylated (TBDMS) in the 2,3,6-O-positions. The beta-CD column with TBDMS substituents in all of the 2,3,6-O-positions was by far the most selective column for the MeSO2-CBs tested. Enantiomers of congeners with 3-MeSO2 substitution were more easily separated than those with 4-MeSO2 substitution. The separation also seemed to be enhanced for congeners with the chlorine atoms on the non-MeSO2-containing ring and clustered on one side of the same ring. The 2,3-di-O-methyl-6-O-TBDMS-beta-CD was found to give somewhat better selectivity than the corresponding gamma-CD, in comparison between the two columns, which were identical in all other respects. Enantioselective analysis of arctic ringed seal (Phoca hispida) and polar bear (Ursus maritimus) adipose tissue revealed a strong dominance of certain enantiomers. For example, the enantiomer ratio (ER) of 3-MeSO2-CB149 was 0.32 and < 0.1 in ringed seal blubber and polar bear fat, respectively. These low ER values are indicative of highly enantioselective formation, enantioselective metabolism, enantioselective transport across cell membranes, or a combination of the three in both species. Comparable results for the enantiomeric analysis of MeSO2-CBs in biotic tissue extracts were obtained using two highly selective mass spectrometric techniques, ion trap mass spectrometry/mass spectrometry and electron capture negative ion low-resolution mass spectrometry. PMID:9751025

  3. Chemometric Profile of Root Extracts of Rhodiola imbricata Edgew. with Hyphenated Gas Chromatography Mass Spectrometric Technique

    PubMed Central

    Tayade, Amol B.; Dhar, Priyanka; Kumar, Jatinder; Sharma, Manu; Chauhan, Rajinder S.; Chaurasia, Om P.; Srivastava, Ravi B.

    2013-01-01

    Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo), belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS) technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S); 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl) phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl); α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful results in

  4. Design and performance of an atmospheric pressure sampling interface for ion-trap/time-of-flight mass spectrometry

    SciTech Connect

    Setz, Patrick D.; Schmitz, Thomas A.; Zenobi, Renato

    2006-02-15

    An ion-trap/time-of-flight mass spectrometer in combination with an atmospheric pressure sampling interface was developed in order to simultaneously profit from the ease of sample handling at ambient pressure, from the storage and accumulation capabilities of an ion trap, and from the acquisition speed and sensitivity of a time-of-flight mass spectrometer. The sampling interface is an intermediate-pressure vacuum manifold that serves to enrich sampled analytes by jet separation with respect to the carrier gas (air) and simultaneously maintain vacuum conditions inside the ion-trap/time-of-flight instrument. Neutral analyte molecules are sampled and later ionized either by electron impact or chemical ionization. Ion accumulation is performed with a rf-only quadrupole ion trap with ground potential on the end caps during storage. For mass analysis, the trap's electrodes serve as a pulsed ion source for the attached linear time-of-flight mass spectrometer. In addition, laser desorbed molecules can also be sampled with this kind of instrument. Successful operation is shown by analyzing volatile substances (aniline, bromobenzene, styrene, and perfluorotributylamine), as well as laser-desorbed organic solids. Figures of merit include a sensitivity of 10 ppm, resolving power of 300 and demonstration of a mass spectrum of laser-desorbed anthracene with a signal-to-noise ratio of 270.

  5. A Linear RFQ Ion Trap for the Enriched Xenon Observatory

    SciTech Connect

    Flatt, B.; Green, M.; Wodin, J.; DeVoe, R.; Fierlinger, P.; Gratta, G.; LePort, F.; Montero Diez, M.; Neilson, R.; O'Sullivan, K.; Pocar, A.; Baussan, E.; Breidenbach, M.; Conley, R.; Fairbank Jr., W.; Farine, J.; Hall, K.; Hallman, D.; Hargrove, C.; Hauger, M.; Hodgson, J.; /Stanford U., Phys. Dept. /Neuchatel U. /SLAC /Colorado State U. /Laurentian U. /Carleton U. /Alabama U.

    2008-01-14

    The design, construction, and performance of a linear radio-frequency ion trap (RFQ) intended for use in the Enriched Xenon Observatory (EXO) are described. EXO aims to detect the neutrinoless double-beta decay of {sup 136}Xe to {sup 136}Ba. To suppress possible backgrounds EXO will complement the measurement of decay energy and, to some extent, topology of candidate events in a Xe filled detector with the identification of the daughter nucleus ({sup 136}Ba). The ion trap described here is capable of accepting, cooling, and confining individual Ba ions extracted from the site of the candidate double-beta decay event. A single trapped ion can then be identified, with a large signal-to-noise ratio, via laser spectroscopy.

  6. Scaling and Suppression of Heating in an Adjustable Ion Trap

    NASA Astrophysics Data System (ADS)

    Olmschenk, Steven; Deslauriers, Louis; Stick, Dan; Hensinger, Winfried; Sterk, Jon; Monroe, Christopher

    2006-05-01

    One of the major hurdles in the realization of large entangled states among trapped ions is anomalous heating of trapped ion motion [1]. We implement a novel rf ion trap featuring moveable electrodes that has enabled a controlled investigation of this motional decoherence. First, we characterize heating as a function of electrode proximity, related to the geometry of noisy potentials on the electrode surface. Second, we cool the electrodes via contact with a liquid nitrogen reservoir and observe that the decoherence rate is suppressed by an order of magnitude. The insight gained through these experiments may have relevance to scaling the ion trap quantum information processor. 1. Q. A. Turchette, et. al., Phys. Rev. A 61, 063418 (2000).

  7. Laser desorption in an ion trap mass spectrometer

    SciTech Connect

    Eiden, G.C.; Cisper, M.E.; Alexander, M.L.; Hemberger, P.H.; Nogar, N.S.

    1993-02-01

    Laser desorption in a ion-trap mass spectrometer shows significant promise for both qualitative and trace analysis. Several aspects of this methodology are discussed in this work. We previously demonstrated the generation of both negative and positive ions by laser desorption directly within a quadrupole ion trap. In the present work, we explore various combinations of d.c., r.f., and time-varying fields in order to optimize laser generated signals. In addition, we report on the application of this method to analyze samples containing compounds such as amines, metal complexes, carbon clusters, and polynuclear aromatic hydrocarbons. In some cases the ability to rapidly switch between positive and negative ion modes provides sufficient specificity to distinguish different compounds of a mixture with a single stage of mass spectrometry. In other experiments, we combined intensity variation studies with tandem mass spectrometry experiments and positive and negative ion detection to further enhance specificity.

  8. Spectroscopy of Argon Excited in an Electron Beam Ion Trap

    SciTech Connect

    Trabert, E

    2005-04-18

    Argon is one of the gases best investigated and most widely used in plasma discharge devices for a multitude of applications that range from wavelength reference standards to controlled fusion experiments. Reviewing atomic physics and spectroscopic problems in various ionization stages of Ar, the past use and future options of employing an electron beam ion trap (EBIT) for better and more complete Ar data in the x-ray, EUV and visible spectral ranges are discussed.

  9. Toward scalable ion traps for quantum information processing

    NASA Astrophysics Data System (ADS)

    Amini, J. M.; Uys, H.; Wesenberg, J. H.; Seidelin, S.; Britton, J.; Bollinger, J. J.; Leibfried, D.; Ospelkaus, C.; VanDevender, A. P.; Wineland, D. J.

    2010-03-01

    In this paper, we report the design, fabrication and preliminary testing of a 150 zone ion trap array built in a 'surface-electrode' geometry microfabricated on a single substrate. We demonstrate the transport of atomic ions between the legs of a 'Y'-type junction and measure the in-situ heating rates for the ions. The trap design demonstrates the use of a basic component design library that can be quickly assembled to form structures optimized for a particular experiment.

  10. Identification of 2-aminothiazolobenzazepine metabolites in human, rat, dog, and monkey microsomes by ion-molecule reactions in linear quadrupole ion trap mass spectrometry.

    PubMed

    Zhang, Minli; Eismin, Ryan; Kenttämaa, Hilkka; Xiong, Hui; Wu, Ye; Burdette, Doug; Urbanek, Rebecca

    2015-03-01

    2-Aminothiazolobenzazepine (2-ATBA), 7-[(1-methyl-1H-pyrazol-4-yl)methyl]-6,7,8,9-tetrahydro-5H-[1,3]thiazolo[4,5-h][3]benzazepin-2-amine, is a D2 partial agonist that has demonstrated antipsychotic effects in a rodent in vivo efficacy model. The metabolite profile showed that 2-ATBA is mainly metabolized by oxidation. However, identification of the oxidation site(s) in the 2-aminothiazole group presents a challenge for the traditional metabolite identification methods such as liquid chromatography/mass spectrometry and NMR due to the lack of unique tandem mass spectrometry fragmentation patterns for ions with the 2-aminothiazole group oxidized at different sites and the lack of stability for purification or reference standard synthesis. We describe the characterization of the oxidized heteroatoms of the 2-aminothiazole group via gas-phase ion-molecule reactions (GPIMR) in a modified linear quadrupole ion trap mass spectrometer. The GPIMR reagents used were dimethyl disulfide, tert-butyl peroxide, and tri(dimethylamino)borane. Each reagent was introduced into the ion trap through the helium line and was allowed to react with the protonated metabolites. The ionic ion-molecule reaction products and their fragmentation profiles were compared with the profiles of the ionic ion-molecule reaction products of protonated reference compounds that had specific heteroatom functionalities. The oxidized 2-aminothiazole metabolite of 2-ATBA showed a similar GPIMR profile to that of the reference compounds with a tertiary N-oxide functionality and distinct from the profiles of the reference compounds with N-aryl hydroxylamine, nitroso, or pyridine N-oxide functionalities. This study demonstrates the feasibility of fingerprinting the chemical nature of oxidized nitrogen functional groups via GPIMR profiling for metabolite structure elucidation. PMID:25547868

  11. Less common applications of monoliths III. Gas chromatography

    PubMed Central

    Svec, Frantisek; Kurganov, Alexander A.

    2008-01-01

    Porous polymer monoliths emerged about two decades ago. Despite this short time, they are finding applications in a variety of fields. In addition to the most common and certainly best known use of this new category of porous media as stationary phases in liquid chromatography, monolithic materials also found their applications in other areas. This review article focuses on monoliths in capillaries designed for separations in gas chromatography. PMID:17645884

  12. Fast screening of anabolic steroids and other banned doping substances in human urine by gas chromatography/tandem mass spectrometry.

    PubMed

    Marcos, J; Pascual, J A; de la Torre, X; Segura, J

    2002-10-01

    A fast and sensitive method for the comprehensive screening of anabolic agents and other banned doping substances using gas chromatography/tandem mass spectrometry (GC/MS/MS) with an external ionization ion trap mass spectrometer is presented. The method takes advantage of the resolving power of MS/MS to eliminate background interferences, thus speeding up the chromatographic analysis. For each compound, different fragmentation reactions were studied and their collision energies optimized to obtain the best sensitivity in terms of their signal-to-noise ratio (S/N). A dramatic reduction in overall analysis time was achieved compared with other common approaches. More than 50 substances could finally be monitored in less than 7.4 min with detection limits (S/N >3) lower than 0.5 ng ml(-1) for most of the compounds with special sensitivity requirements according to the International Olympic Committee (IOC). A validation procedure for qualitative analysis was performed. The selectivity of the method showed that no interfering peaks were observed at the retention time of the analytes. Good intermediate precision, below 25% for most of the compounds, and robustness were observed. The optimized method was successfully applied to analyse more than 100 real human urine samples with optimum sensitivity and specificity rates. PMID:12375280

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

    NASA Technical Reports Server (NTRS)

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

    2002-01-01

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

  14. PROCESS GAS CHROMATOGRAPHY STUDY OF A SELEXOL ACID GAS REMOVAL SYSTEM

    EPA Science Inventory

    The report gives results of continuous compositional monitoring by process gas chromatography (GC) for three gas streams associated with the Selexol acid gas removal system at the Bi-Gas pilot plant in Homer City, PA. Data were obtained from the inlet and outlet streams of the Se...

  15. Reactions of vinyl chloride and methanol in a quadrupole ion trap mass spectrometer during VOC analysis

    SciTech Connect

    Bian, L.; Alley, E.G.; Lynn, B.C. Jr.

    1999-05-01

    A reaction between vinyl chloride and the solvent (methanol) was observed during volatile organic compound (VOC) analysis on a gas chromatograph/quadrupole ion trap mass spectrometer (GC/MS). A chromatographic peak at a retention time consistent with vinyl chloride produced a mass spectrum without the characteristic chlorine isotope ions m/z 62 and 64 but instead contained an apparent molecular ion, m/z 58. The m/z 58 ion is not found in the reference spectrum of vinyl chloride. This spectrum was observed when methanol was used as solvent in internal standard, surrogate standard, or analyte solutions. Subsequent VOC standard analysis indicated that the abundance of the m/z 58 ion was directly proportional to the amount of vinyl chloride in the water samples. The correct spectrum for vinyl chloride was observed when no methanol was added. From these experiments, the authors concluded that a reaction was occurring between the vinyl chloride and methanol in the ion trap producing a new species with a molecular ion at m/z 58. When ethanol was used as the solvent for the internal standard solution or surrogate standard, a correct spectrum of vinyl chloride was obtained.

  16. Theoretical Study of Dual-Direction Dipolar Excitation of Ions in Linear Ion Traps

    NASA Astrophysics Data System (ADS)

    Dang, Qiankun; Xu, Fuxing; Wang, Liang; Huang, Xiaohua; Dai, Xinhua; Fang, Xiang; Wang, Rizhi; Ding, Chuan-Fan

    2016-04-01

    The ion enhanced activation and collision-induced dissociation (CID) by simultaneous dipolar excitation of ions in the two radial directions of linear ion trap (LIT) have been recently developed and tested by experiment. In this work, its detailed properties were further studied by theoretical simulation. The effects of some experimental parameters such as the buffer gas pressure, the dipolar excitation signal phases, power amplitudes, and frequencies on the ion trajectory and energy were carefully investigated. The results show that the ion activation energy can be significantly increased by dual-direction excitation using two identical dipolar excitation signals because of the addition of an excitation dimension and the fact that the ion motion radius related to ion kinetic energy can be greater than the field radius. The effects of higher-order field components, such as dodecapole field on the performance of this method are also revealed. They mainly cause ion motion frequency shift as ion motion amplitude increases. Because of the frequency shift, there are different optimized excitation frequencies in different LITs. At the optimized frequency, ion average energy is improved significantly with relatively few ions lost. The results show that this method can be used in different kinds of LITs such as LIT with 4-fold symmetric stretch, linear quadrupole ion trap, and standard hyperbolic LIT, which can significantly increase the ion activation energy and CID efficiency, compared with the conventional method.

  17. Theoretical Study of Dual-Direction Dipolar Excitation of Ions in Linear Ion Traps.

    PubMed

    Dang, Qiankun; Xu, Fuxing; Wang, Liang; Huang, Xiaohua; Dai, Xinhua; Fang, Xiang; Wang, Rizhi; Ding, Chuan-Fan

    2016-04-01

    The ion enhanced activation and collision-induced dissociation (CID) by simultaneous dipolar excitation of ions in the two radial directions of linear ion trap (LIT) have been recently developed and tested by experiment. In this work, its detailed properties were further studied by theoretical simulation. The effects of some experimental parameters such as the buffer gas pressure, the dipolar excitation signal phases, power amplitudes, and frequencies on the ion trajectory and energy were carefully investigated. The results show that the ion activation energy can be significantly increased by dual-direction excitation using two identical dipolar excitation signals because of the addition of an excitation dimension and the fact that the ion motion radius related to ion kinetic energy can be greater than the field radius. The effects of higher-order field components, such as dodecapole field on the performance of this method are also revealed. They mainly cause ion motion frequency shift as ion motion amplitude increases. Because of the frequency shift, there are different optimized excitation frequencies in different LITs. At the optimized frequency, ion average energy is improved significantly with relatively few ions lost. The results show that this method can be used in different kinds of LITs such as LIT with 4-fold symmetric stretch, linear quadrupole ion trap, and standard hyperbolic LIT, which can significantly increase the ion activation energy and CID efficiency, compared with the conventional method. Graphical Abstract ᅟ. PMID:26810433

  18. Gas chromatography/matrix-isolation apparatus

    DOEpatents

    Reedy, Gerald T.

    1986-01-01

    A gas-sample collection device provides matrix isolation of individual gas bands from a gas chromatographic separation and for the spectroscopic analysis of the individual sample bands. The device includes a vacuum chamber containing a rotatably supported, specular carousel having at least one reflecting surface for holding a sample deposited thereon. A gas inlet is provided for depositing a mixture of sample and matrix material on the reflecting surface which is maintained at a sufficiently low temperature to cause solidification. A first parabolic mirror directs an incident beam of electromagnetic radiation, such as in the infrared (IR) spectrum, from a source onto the sample/matrix mixture while a second parabolic mirror directs a second beam of electromagnetic radiation reflected by the specular surface to an IR spectrometer for determining the absorption spectra of the sample material deposited on the reflecting surface. The pair of off-axis parabolic mirrors having a common focal point are positioned outside of the vacuum chamber and may be displaced in combination for improved beam positioning and alignment. The carousel is provided with an aperture for each reflecting surface to facilitate accurate positioning of the incident beam relative to the gas-samples under analysis. Improved gas-sample deposition is insured by the use of a long focal length stereomicroscope positioned outside of the vacuum chamber for monitoring sample formation through a window, while the sample collector is positioned outside of the zone bounded by the incident and reflected electromagnetic beams for improved sample access and monitoring.

  19. An ion trap built with photonic crystal fibre technology

    SciTech Connect

    Lindenfelser, F. Keitch, B.; Kienzler, D.; Home, J. P.; Bykov, D.; Uebel, P.; Russell, P. St. J.

    2015-03-15

    We demonstrate a surface-electrode ion trap fabricated using techniques transferred from the manufacture of photonic-crystal fibres. This provides a relatively straightforward route for realizing traps with an electrode structure on the 100 micron scale with high optical access. We demonstrate the basic functionality of the trap by cooling a single ion to the quantum ground state, allowing us to measure a heating rate from the ground state of 787 ± 24 quanta/s. Variation of the fabrication procedure used here may provide access to traps in this geometry with trap scales between 100 μm and 10 μm.

  20. Measurement of femtosecond atomic lifetimes using ion traps

    NASA Astrophysics Data System (ADS)

    Träbert, Elmar

    2014-01-01

    Two types of experiment are described that both employ an electron beam ion trap for the production of highly charged ion species with the aim of then measuring atomic level lifetimes in the femtosecond range. In one experiment (done by Beiersdorfer et al. some time ago), the lifetime measurement depends on the associated line broadening. In a recent string of experiments at Linac Coherent Light Source Stanford, the HI-LIGHT collaboration employed pump-probe excitation using the FEL as a short-pulse X-ray laser.

  1. New ion trap for atomic frequency standard applications

    NASA Technical Reports Server (NTRS)

    Prestage, J. D.; Dick, G. J.; Maleki, L.

    1989-01-01

    A novel linear ion trap that permits storage of a large number of ions with reduced susceptibility to the second-order Doppler effect caused by the radio frequency (RF) confining fields has been designed and built. This new trap should store about 20 times the number of ions a conventional RF trap stores with no corresponding increase in second-order Doppler shift from the confining field. In addition, the sensitivity of this shift to trapping parameters, i.e., RF voltage, RF frequency, and trap size, is greatly reduced.

  2. Progress Report on the Improved Linear Ion Trap Physics Package

    NASA Technical Reports Server (NTRS)

    Prestage, John D.

    1995-01-01

    This article describes the first operational results from the extended linear ion trap frequency standard now being developed at JPL. This new design separates the state selection/interrogation region from the more critical microwave resonance region where the multiplied local oscillator (LO) signal is compared to the stable atomic transition. Hg+ ions have been trapped, shuttled back and forth between the resonance and state selection traps. In addition, microwave transitions between the Hg+ clock levels have been driven in the resonance trap and detected in the state selection trap.

  3. An ion trap built with photonic crystal fibre technology.

    PubMed

    Lindenfelser, F; Keitch, B; Kienzler, D; Bykov, D; Uebel, P; Schmidt, M A; Russell, P St J; Home, J P

    2015-03-01

    We demonstrate a surface-electrode ion trap fabricated using techniques transferred from the manufacture of photonic-crystal fibres. This provides a relatively straightforward route for realizing traps with an electrode structure on the 100 micron scale with high optical access. We demonstrate the basic functionality of the trap by cooling a single ion to the quantum ground state, allowing us to measure a heating rate from the ground state of 787 ± 24 quanta/s. Variation of the fabrication procedure used here may provide access to traps in this geometry with trap scales between 100 μm and 10 μm. PMID:25832211

  4. Note: Ion source design for ion trap systems

    NASA Astrophysics Data System (ADS)

    Noriega, J. R.; Quevedo, M.; Gnade, B.; Vasselli, J.

    2013-06-01

    A small plasma (glow discharge) based ion source and circuit are described in this work. The ion source works by producing a high voltage pulsed discharge between two electrodes in a pressure range of 50-100 mTorr. A third mesh electrode is used for ion extraction. The electrodes are small stainless steel screws mounted in a MACOR ionization chamber in a linear arrangement. The electrode arrangement is driven by a circuit, design for low power operation. This design is a proof of concept intended for applications on small cylindrical ion traps.

  5. Experimental demonstration of a surface-electrode multipole ion trap

    NASA Astrophysics Data System (ADS)

    Maurice, Mark; Allen, Curtis; Green, Dylan; Farr, Andrew; Burke, Timothy; Hilleke, Russell; Clark, Robert

    2015-08-01

    We report on the design and experimental characterization of a surface-electrode multipole ion trap. Individual microscopic sugar particles are confined in the trap. The trajectories of driven particle motion are compared with a theoretical model, both to verify qualitative predictions of the model and to measure the charge-to-mass ratio of the confined particle. The generation of harmonics of the driving frequency is observed as a key signature of the nonlinear nature of the trap. We remark on possible applications of our traps, including to mass spectrometry.

  6. Electron beam ion source and electron beam ion trap (invited)

    SciTech Connect

    Becker, Reinard; Kester, Oliver

    2010-02-15

    The electron beam ion source (EBIS) and its trap variant [electron beam ion trap (EBIT)] celebrated their 40th and 20th anniversary, respectively, at the EBIS/T Symposium 2007 in Heidelberg. These technologically challenging sources of highly charged ions have seen a broad development in many countries over the last decades. In contrast to most other ion sources the recipe of improvement was not ''sorcery'' but a clear understanding of the physical laws and obeying the technological constraints. This review will report important achievements of the past as well as promising developments in the future.

  7. Design Optimization for Anharmonic Linear Surface-Electrode Ion Trap

    NASA Astrophysics Data System (ADS)

    Liu, Wei; Chen, Shu-Ming; Chen, Ping-Xing; Wu, Wei

    2014-11-01

    An accurate and rapid method is proposed to optimize anharmonic linear surface-electrode ion trap design. Based on the method, we analyze the impact of the architectural parameters, including the width, number, and applied voltage of prerequisite active electrodes, on the number and spacing of trapped ions. Sets of optimal anharmonic trap design are given. Then the optimal designs are verified by using an ant colony optimization algorithm. The results show that the maximum ion position errors and maximum ion spacing errors are less than 1 μm up to 80. The mean of the maximum errors is nearly linear with respect to the number of trapped ions.

  8. Ion collision cross section analyses in quadrupole ion traps using the filter diagonalization method: a theoretical study.

    PubMed

    Jiang, Ting; He, Miyi; Guo, Dan; Zhai, Yanbing; Xu, Wei

    2016-04-28

    Previously, we have demonstrated the feasibility of measuring ion collision cross sections (CCSs) within a quadrupole ion trap by performing time-frequency analyses of simulated ion trajectories. In this study, an improved time-frequency analysis method, the filter diagonalization method (FDM), was applied for data analyses. Using the FDM, high resolution could be achieved in both time- and frequency-domains when calculating ion time-frequency curves. Owing to this high-resolution nature, ion-neutral collision induced ion motion frequency shifts were observed, which further cause the intermodulation of ion trajectories and thus accelerate image current attenuation. Therefore, ion trap operation parameters, such as the ion number, high-order field percentage and buffer gas pressure, were optimized for ion CCS measurements. Under optimized conditions, simulation results show that a resolving power from 30 to more than 200 could be achieved for ion CCS measurements. PMID:27066889

  9. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    ERIC Educational Resources Information Center

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-01-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal…

  10. IMPROVED FAST GAS CHROMATOGRAPHY FOR FAME ANALYSIS OF BACTERIA

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Bacteria are frequently identified by fatty acid analysis. We previously reported on methods to speed up sample preparation and gas chromatography, resulting in greatly improved speed and throughput (Buyer, 2002). In this paper we demonstrate that further reductions in chromatographic retention time...

  11. Optimization of strawberry volatile sampling by direct gas chromatography olfactometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The aim of this work was to choose a suitable sampling headspace technique to study ‘Festival’ aroma, the main strawberry cultivar grown in Florida. For that, the aromatic quality of extracts from different headspace techniques was evaluated using direct gas chromatography-olfactometry (D-GC-O), a s...

  12. Enthalpy of Vaporization by Gas Chromatography: A Physical Chemistry Experiment

    ERIC Educational Resources Information Center

    Ellison, Herbert R.

    2005-01-01

    An experiment is conducted to measure the enthalpy of vaporization of volatile compounds like methylene chloride, carbon tetrachloride, and others by using gas chromatography. This physical property was measured using a very tiny quantity of sample revealing that it is possible to measure the enthalpies of two or more compounds at the same time.

  13. Highly crosslinked silicon polymers for gas chromatography columns

    NASA Technical Reports Server (NTRS)

    Shen, Thomas C. (Inventor)

    1994-01-01

    A new highly crosslinked silicone polymer particle for gas chromatography application and a process for synthesizing such copolymer are described. The new copolymer comprises vinyltriethoxysilane and octadecyltrichlorosilane. The copolymer has a high degree of crosslinking and a cool balance of polar to nonpolar sites in the porous silicon polymer assuring fast separation of compounds of variable polarity.

  14. Specialized Gas Chromatography--Mass Spectrometry Systems for Clinical Chemistry.

    ERIC Educational Resources Information Center

    Gochman, Nathan; And Others

    1979-01-01

    A discussion of the basic design and characteristics of gas chromatography-mass spectrometry systems used in clinical chemistry. A comparison of three specific systems: the Vitek Olfax IIA, Hewlett-Packard HP5992, and Du Pont DP-102 are included. (BB)

  15. An application of gas chromatography to planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Oyama, V.

    1974-01-01

    A gas chromatography developed for the Viking experiment is described. The instrument is designed to measure gases in planetary atmospheres and head space in a chamber. It is hoped that the chromatograph will also measure any biological activity present in these environments.

  16. Characterization of the chemical composition of white chrysanthemum flowers of Hangzhou by using high-performance ion trap mass spectrometry.

    PubMed

    Zhou, Xiahui; Chen, Xiaocheng; Wu, Xin; Cao, Gang; Zhang, Junjie

    2016-04-01

    In this study, high-performance liquid chromatography coupled with amaZon SL high-performance ion trap mass spectrometry was used to analyze the target components in white chrysanthemum flowers of Hangzhou. Twenty-one components were detected and identified in both white chrysanthemum flowers of Hangzhou samples by using target compound analysis. Furthermore, seven new compounds in white chrysanthemum flowers of Hangzhou were found and identified by analyzing the fragment ion behavior in the mass spectra. The established method can be expedient for the global quality investigation of complex components in herbal medicines and food. PMID:26843262

  17. Gas chromatography/matrix-isolation apparatus

    DOEpatents

    Reedy, G.T.

    1986-06-10

    A gas-sample collection device provides matrix isolation of individual gas bands from a gas chromatographic separation and for the spectroscopic analysis of the individual sample bands. The device includes a vacuum chamber containing a rotatably supported, specular carousel having at least one reflecting surface for holding a sample deposited thereon. A gas inlet is provided for depositing a mixture of sample and matrix material on the reflecting surface which is maintained at a sufficiently low temperature to cause solidification. A first parabolic mirror directs an incident beam of electromagnetic radiation, such as in the infrared (IR) spectrum, from a source onto the sample/matrix mixture while a second parabolic mirror directs a second beam of electromagnetic radiation reflected by the specular surface to an IR spectrometer for determining the absorption spectra of the sample material deposited on the reflecting surface. The pair of off-axis parabolic mirrors having a common focal point are positioned outside of the vacuum chamber and may be displaced in combination for improved beam positioning and alignment. The carousel is provided with an aperture for each reflecting surface to facilitate accurate positioning of the incident beam relative to the gas-samples under analysis. Improved gas-sample deposition is insured by the use of a long focal length stereomicroscope positioned outside of the vacuum chamber for monitoring sample formation through a window, while the sample collector is positioned outside of the zone bounded by the incident and reflected electromagnetic beams for improved sample access and monitoring. 10 figs.

  18. MEMS-based arrays of micro ion traps for quantum simulation scaling.

    SciTech Connect

    Berkeland, Dana J.; Blain, Matthew Glenn; Jokiel, Bernhard, Jr.

    2006-11-01

    In this late-start Tier I Seniors Council sponsored LDRD, we have designed, simulated, microfabricated, packaged, and tested ion traps to extend the current quantum simulation capabilities of macro-ion traps to tens of ions in one and two dimensions in monolithically microfabricated micrometer-scaled MEMS-based ion traps. Such traps are being microfabricated and packaged at Sandia's MESA facility in a unique tungsten MEMS process that has already made arrays of millions of micron-sized cylindrical ion traps for mass spectroscopy applications. We define and discuss the motivation for quantum simulation using the trapping of ions, show the results of efforts in designing, simulating, and microfabricating W based MEMS ion traps at Sandia's MESA facility, and describe is some detail our development of a custom based ion trap chip packaging technology that enables the implementation of these devices in quantum physics experiments.

  19. Ion Trap Array-Based Systems And Methods For Chemical Analysis

    DOEpatents

    Whitten, William B [Oak Ridge, TN; Ramsey, J Michael [Knoxville, TN

    2005-08-23

    An ion trap-based system for chemical analysis includes an ion trap array. The ion trap array includes a plurality of ion traps arranged in a 2-dimensional array for initially confining ions. Each of the ion traps comprise a central electrode having an aperture, a first and second insulator each having an aperture sandwiching the central electrode, and first and second end cap electrodes each having an aperture sandwiching the first and second insulator. A structure for simultaneously directing a plurality of different species of ions out from the ion traps is provided. A spectrometer including a detector receives and identifies the ions. The trap array can be used with spectrometers including time-of-flight mass spectrometers and ion mobility spectrometers.

  20. Is the Penning Ion Trap Suitable for Quantum Computation?

    NASA Astrophysics Data System (ADS)

    Bollinger, J. J.; Kriesel, J. M.; Itano, W. M.; Mitchell, T. B.

    2001-10-01

    There is a great deal of interest in finding a physical system which can perform computations through quantum unitary operations and be scaled to large numbers of qubits. rf ion traps have been used in pioneering experiments on a few qubits. The Penning ion trap has some potential advantages compared to the rf trap. In rf traps, heating and decoherence rates of ion motional states have been observed to scale inversely with the size of the electrodes. Penning traps can have large electrodes while still retaining the large (5-10 MHz) motional frequencies required for quantum logic operations. This is because large static fields are more easily generated than large amplitude rf fields. Addressing of individual ions in the Penning trap is complicated by the plasma rotation, but should be possible with crystallized, planar plasmas controlled by a combination of rotating fields (a ``hard disk" geometry). We will discuss the pros and cons as well as some initial experiments to investigate the suitability of the Penning trap for quantum computation.

  1. Ball-grid array architecture for microfabricated ion traps

    SciTech Connect

    Guise, Nicholas D. Fallek, Spencer D.; Stevens, Kelly E.; Brown, K. R.; Volin, Curtis; Harter, Alexa W.; Amini, Jason M.; Higashi, Robert E.; Lu, Son Thai; Chanhvongsak, Helen M.; Nguyen, Thi A.; Marcus, Matthew S.; Ohnstein, Thomas R.; Youngner, Daniel W.

    2015-05-07

    State-of-the-art microfabricated ion traps for quantum information research are approaching nearly one hundred control electrodes. We report here on the development and testing of a new architecture for microfabricated ion traps, built around ball-grid array (BGA) connections, that is suitable for increasingly complex trap designs. In the BGA trap, through-substrate vias bring electrical signals from the back side of the trap die to the surface trap structure on the top side. Gold-ball bump bonds connect the back side of the trap die to an interposer for signal routing from the carrier. Trench capacitors fabricated into the trap die replace area-intensive surface or edge capacitors. Wirebonds in the BGA architecture are moved to the interposer. These last two features allow the trap die to be reduced to only the area required to produce trapping fields. The smaller trap dimensions allow tight focusing of an addressing laser beam for fast single-qubit rotations. Performance of the BGA trap as characterized with {sup 40}Ca{sup +} ions is comparable to previous surface-electrode traps in terms of ion heating rate, mode frequency stability, and storage lifetime. We demonstrate two-qubit entanglement operations with {sup 171}Yb{sup +} ions in a second BGA trap.

  2. Collisional activation with random noise in ion trap mass spectrometry

    SciTech Connect

    McLuckey, S.A.; Goeringer, D.E.; Glish, G.L.

    1992-07-01

    Random noise applied to the end caps of a quadrupole ion trap is shown to be an effective means for the collisional activation of trapped ions independent of mass/charge ratio and number of ions. This technique is compared and contrasted with conventional single-frequency collisional activation for the molecular ion of N,N-dimethylaniline, protonated cocaine, the molecular anion of 2,4,6-trinitrotoluene, and doubly protonated neuromedin U-8. Collisional activation with noise tends to produce more extensive fragmentation than the conventional approach due to the fact that product ions are also kinetically excited in the noise experiment. The efficiency of the noise experiment in producing detectable product ions relative to the conventional approach ranges from being equivalent to being a factor of 3 less efficient. Furthermore, discrimination against low mass/charge product ions is apparent in the data from multiply charged biomolecules. Nevertheless, collisional activation with random noise provides a very simple means for overcoming problems associated with the dependence of single-frequency collisional activation on mass/charge ratio and the number of ions in the ion trap. 45 refs., 7 figs.

  3. Charged-Particle Bean Transport for Ion Trapping Experiments.

    NASA Astrophysics Data System (ADS)

    Raichle, Brian W.; Wingfield, Love M.

    2001-11-01

    Electrostatic Einsel lenses are being developed for beam transport for use in two distinct metastable atomic lifetime experiments using two separate rf-ion traps. Each system has been modeled using Simion software, and the lenses have been designed from commercially available eV-parts. The first application is part of an electron gun source. Electrons are produced by a conventional dispenser cathode and are transported 25 cm to the trap. The design goal is to create a beam divergence to fully illuminate the active trap volume, and to provide tunable electron energies from 50 to 500 eV. The second application is to transport ions 1 m from a laser ablation ion source to an rf ion trap. Laser ablation involves essentially boiling ions from a solid target with intense laser pulses. Here, the design goal is to maximize flux by maximizing the solid angle of acceptance to the trap, minimize radial velocity, and minimize the spread in axial velocity. Development of a laser ablation ion source external to the trap volume will allow a very low base pressure in the trap region, which will make possible the study of species with lifetimes approaching 1 s. In addition, laser ablation will produce intermediately-charged ions from non-conductive solid targets.

  4. Laser desorption lamp ionization source for ion trap mass spectrometry.

    PubMed

    Wu, Qinghao; Zare, Richard N

    2015-01-01

    A two-step laser desorption lamp ionization source coupled to an ion trap mass spectrometer (LDLI-ITMS) has been constructed and characterized. The pulsed infrared (IR) output of an Nd:YAG laser (1064 nm) is directed to a target inside a chamber evacuated to ~15 Pa causing desorption of molecules from the target's surface. The desorbed molecules are ionized by a vacuum ultraviolet (VUV) lamp (filled with xenon, major wavelength at 148 nm). The resulting ions are stored and detected in a three-dimensional quadrupole ion trap modified from a Finnigan Mat LCQ mass spectrometer operated at a pressure of ≥ 0.004 Pa. The limit of detection for desorbed coronene molecules is 1.5 pmol, which is about two orders of magnitude more sensitive than laser desorption laser ionization mass spectrometry using a fluorine excimer laser (157 nm) as the ionization source. The mass spectrum of four standard aromatic compounds (pyrene, coronene, rubrene and 1,4,8,11,15,18,22,25-octabutoxy-29H,31H-phthalocyanine (OPC)) shows that parent ions dominate. By increasing the infrared laser power, this instrument is capable of detecting inorganic compounds. PMID:25601688

  5. "Fast Excitation" CID in Quadrupole Ion Trap Mass Spectrometer

    SciTech Connect

    Murrell, J.; Despeyroux, D.; Lammert, Stephen {Steve} A; Stephenson Jr, James {Jim} L; Goeringer, Doug

    2003-01-01

    Collision-induced dissociation (CID) in a quadrupole ion trap mass spectrometer is usually performed by applying a small amplitude excitation voltage at the same secular frequency as the ion of interest. Here we disclose studies examining the use of large amplitude voltage excitations (applied for short periods of time) to cause fragmentation of the ions of interest. This process has been examined using leucine enkephalin as the model compound and the motion of the ions within the ion trap simulated using ITSIM. The resulting fragmentation information obtained is identical with that observed by conventional resonance excitation CID. ''Fast excitation'' CID deposits (as determined by the intensity ratio of the a{sub 4}/b{sub 4} ion of leucine enkephalin) approximately the same amount of internal energy into an ion as conventional resonance excitation CID where the excitation signal is applied for much longer periods of time. The major difference between the two excitation techniques is the higher rate of excitation (gain in kinetic energy) between successive collisions with helium atoms with ''fast excitation'' CID as opposed to the conventional resonance excitation CID. With conventional resonance excitation CID ions fragment while the excitation voltage is still being applied whereas for ''fast excitation'' CID a higher proportion of the ions fragment in the ion cooling time following the excitation pulse. The fragmentation of the (M + 17H){sup 17+} of horse heart myoglobin is also shown to illustrate the application of ''fast excitation'' CID to proteins.

  6. A Scalable Microfabricated Ion Trap for Quantum Information Processing

    NASA Astrophysics Data System (ADS)

    Maunz, Peter; Haltli, Raymond; Hollowell, Andrew; Lobser, Daniel; Mizrahi, Jonathan; Rembetski, John; Resnick, Paul; Sterk, Jonathan D.; Stick, Daniel L.; Blain, Matthew G.

    2016-05-01

    Trapped Ion Quantum Information Processing (QIP) relies on complex microfabricated trap structures to enable scaling of the number of quantum bits. Building on previous demonstrations of surface-electrode ion traps, we have designed and characterized the Sandia high-optical-access (HOA-2) microfabricated ion trap. This trap features high optical access, high trap frequencies, low heating rates, and negligible charging of dielectric trap components. We have observed trap lifetimes of more than 100h, measured trap heating rates for ytterbium of less than 40quanta/s, and demonstrated shuttling of ions from a slotted to an above surface region and through a Y-junction. Furthermore, we summarize demonstrations of high-fidelity single and two-qubit gates realized in this trap. Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy's National Nuclear Security Administration under Contract DE-AC04-94AL85000. This work was supported by the Intelligence Advanced Research Projects Activity (IARPA).

  7. Quantitative determination of hydrogen in solids by gas chromatography.

    PubMed

    Addach, H; Berçot, P; Wery, M; Rezrazi, M

    2004-11-19

    Processes such as electroplating or acid cleaning are notorious causes of post-processing failure through hydrogen embrittlement. So, the determination of amounts of hydrogen in metals is of great importance. An analysis method for investigation of H content in solids has been established based on hot extraction and gas chromatography system. Hot extraction in inert gas enables complete and/or partial removal of the hydrogen from the samples. A gas chromatography system is used to determine quantitatively the amount of thermally desorbed hydrogen. An investigation of the baking operating conditions is made of the hydrogen desorption rate of zinc-plated steel parts. Then, an analysis of the polarisation conditions upon chromium electroplating is given. PMID:15584242

  8. Multiplex gas chromatography for use in space craft

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.

    1985-01-01

    Gas chromatography is a powerful technique for the analysis of gaseous mixtures. Some limitations in this technique still exist which can be alleviated with multiplex gas chromatography (MGC). In MGC, rapid multiple sample injections are made into the column without having to wait for one determination to be finished before taking a new sample. The resulting data must then be reduced using computational methods such as cross correlation. In order to efficiently perform multiplexgas chromatography, experiments in the laboratory and on board future space craft, skills, equipment, and computer software were developed. Three new techniques for modulating, i.e., changing, sample concentrations were demonstrated by using desorption, decomposition, and catalytic modulators. In all of them, the need for a separate gas stream as the carrier was avoided by placing the modulator at the head of the column to directly modulate a sample stream. Finally, the analysis of an environmental sample by multiplex chromatography was accomplished by employing silver oxide to catalytically modulate methane in ambient air.

  9. Linear ion trap for second-order Doppler shift reduction in frequency standard applications

    NASA Technical Reports Server (NTRS)

    Prestage, John D.; Janik, Gary R.; Dick, G. John; Maleki, Lute

    1990-01-01

    The authors have designed and are presently testing a novel linear ion trap that permits storage of a large number of ions with reduced susceptibility to the second-order Doppler effect caused by the RF confining fields. This new trap should store about 20 times the number of ions as a conventional RF trap with no corresponding increase in second-order Doppler shift from the confining field. In addition, the sensitivity of this shift to trapping parameters, i.e., RF voltage, RF frequency, and trap size, is greatly reduced. The authors have succeeded in trapping mercury ions and xenon ions in the presence of helium buffer gas. Trap times as long as 2000 s have been measured.

  10. Multiple-injection high-throughput gas chromatography analysis.

    PubMed

    Schafer, Wes; Wang, Heather; Welch, Christopher J

    2016-08-01

    Multiple-injection techniques have been shown to be a simple way to perform high-throughput analysis where the entire experiment resides in a single chromatogram, simplifying the data analysis and interpretation. In this study, multiple-injection techniques are applied to gas chromatography with flame ionization detection and mass detection to significantly increase sample throughput. The unique issues of implementing a traditional "Fast" injection mode of multiple-injection techniques with gas chromatography and mass spectrometry are discussed. Stacked injections are also discussed as means to increase the throughput of longer methods where mass detection is unable to distinguish between analytes of the same mass and longer retentions are required to resolve components of interest. Multiple-injection techniques are shown to increase instrument throughput by up to 70% and to simplify data analysis, allowing hits in multiple parallel experiments to be identified easily. PMID:27292909

  11. Photodissociation Spectroscopy of Ca^+-H_2O in the Temperature-Variable Ion Trap

    NASA Astrophysics Data System (ADS)

    Ishikawa, Haruki; Eguchi, Toru; Nakano, Takumi; Fujihara, Akimasa; Fuke, Kiyokazu

    2011-06-01

    In the last two decades, developments of infrared spectroscopy and theoretical calculations on gas-phase molecular clusters have revealed detailed solvation structures of various systems, especially of hydrogen-bonded systems. One of the remained problems in studies on microscopic solvation or hydration is a temperature dependence of solvation structures. Lisy and coworkers succeeded in interpreting the hydration structures of alkali metal ions by taking temperature- or entropic effect. They utilized Ar vaporization to cool down the temperature of clusters. Another method for controlling temperature of cluster ions is a buffer gas cooling in an ion trap. In the present study, we have measured photodissociation spectra of Ca^+-H_2O in our temperature-variable ion trap In the present study, we examined the temperature of the Ca^+-H_2O in the trap by simulating the rotational profile of the 0-0 band of the ^2B_1 - ^2A_1 transition. The observed rotational profile is similar to that reported by Duncan and coworkers. By changing the trap period from 10 ms to 40 ms, it was confirmed that the trap period of 10 ms is sufficient to get temperature equilibrium in our experimental condition. Details of the experimental results will be presented in the paper. D. J. Miller, J. M. Lisy J. Am. Chem. Soc. 130, 15393 (2008). A. Fujihara, et al. J. Phys. Chem. A 112, 1457 (2008) A. Fujihara, et al. J. Phys. Chem. A 113, 8169 (2009). C. T. Scurlock, S. H. Pullins, J. E. Reddic, M. A. Duncan J. Chem. Phys. 104, 4591 (1996).

  12. Field-free junctions for surface electrode ion traps

    NASA Astrophysics Data System (ADS)

    Jordens, Robert; Schmied, R.; Blain, M. G.; Leibfried, D.; Wineland, D.

    2015-05-01

    Intersections between transport guides in a network of RF ion traps are a key ingredient to many implementations of scalable quantum information processing with trapped ions. Several junction architectures demonstrated so far are limited by varying radial secular frequencies, a reduced trap depth, or a non-vanishing RF field along the transport channel. We report on the design and progress in implementing a configurable microfabricated surface electrode Y-junction that employs switchable RF electrodes. An essentially RF-field-free pseudopotential guide between any two legs of the junction can be established by applying RF potential to a suitable pair of electrodes. The transport channel's height above the electrodes, its depth and radial curvature are constant to within 15%. Supported by IARPA, Sandia, NSA, ONR, and the NIST Quantum Information Program.

  13. Progress Towards Quantum Simulation Using Micro-fabricated Ion Traps

    NASA Astrophysics Data System (ADS)

    Wright, K.; Ji, G.; Rickerd, C.; Collins, K.; Monroe, C.

    2015-05-01

    We report on current experimental progress towards using a surface electrode trap for quantum simulation. We use a micro-fabricated trap developed collaboratively between the Georgia Tech Research Institute (GTRI) and Honeywell International known as the Ball Grid Array (BGA) trap. This trap features 96 electrodes for fine control of the DC potential as well as a small footprint allowing for tight focusing of interaction lasers. We discuss the experimental system which utilizes the BGA trap, loading of Yb171 ions in this trap, and deterministic loading of chains of five or more ions. We hope to take advantage of the features of this new trap architecture in order to perform a small scale Boson Sampling experiment. This work is performed in collaboration with the GTRI Ion Trap Group and supported by ARO with funding from the IARPA MQCO program, and the AFOSR STTR on Atom Trap Chips.

  14. Ion-trapping and end-capping in ionic polymerizations

    SciTech Connect

    Penczek, S.

    1993-12-31

    Ion-trapping, developed in this laboratory, involves both vinyl and ring-opening polymerizations, anionic and cationic. Originally it was elaborated for cationic ring-opening polymerization and involved reaction of phosphines (mostly triphenylphosphine) with onium ions, like oxonium ions in the polymerization of cyclic ethers. The same method has more recently been used for the cationic polymerization of vinyl ethers, allowing not only to determine the total concentration of the growing species by {sup 31}P-NMR but also to study the stereochemistry of the chain end by the same method. In the anionic ring-opening polymerization diphenylchlorophosphate was applied. It reacts quantitatively with alcoholate, thiolate, and carboxylate anions. More recently diphenylchlorophosphine was successfully used to determine the concentration and structure of the chain ends in the anionic polymerization of styrene, butadiene, isoprene as well as their mixtures.

  15. Laser ablation loading of a surface-electrode ion trap

    SciTech Connect

    Leibrandt, David R.; Clark, Robert J.; Labaziewicz, Jaroslaw; Antohi, Paul; Bakr, Waseem; Brown, Kenneth R.; Chuang, Isaac L.

    2007-11-15

    We demonstrate loading of {sup 88}Sr{sup +} ions by laser ablation into a mm-scale surface-electrode ion trap. The laser used for ablation is a pulsed, frequency-tripled Nd:YAG with pulse energies of 1-10 mJ and durations of 4 ns. An additional laser is not required to photoionize the ablated material. The efficiency and lifetime of several candidate materials for the laser ablation target are characterized by measuring the trapped ion fluorescence signal for a number of consecutive loads. Additionally, laser ablation is used to load traps with a trap depth (40 meV) below where electron impact ionization loading is typically successful (> or approx. 500 meV)

  16. Compact toroidal ion-trap design and optimization

    SciTech Connect

    Madsen, M. J.; Gorman, C. H.

    2010-10-15

    We present the design of a type of compact toroidal, or 'halo', ion trap. Such traps may be useful for mass spectrometry, studying small Coulomb cluster rings, quantum-information applications, or other quantum simulations where a ring topology is of interest. We present results from a Monte Carlo optimization of the trap design parameters using finite-element analysis simulations that minimize higher-order anharmonic terms in the trapping pseudopotential, while maintaining complete control over ion placement at the pseudopotential node in three dimensions using static bias fields. These simulations are based on a practical electrode design using readily available parts, yet can be easily scaled to any size trap with similar electrode spacings. We also derive the conditions for a crystal structure transition for two ions in the compact halo trap, the first nontrivial transition for Coulomb crystals in this geometry.

  17. The determination of soil moisture by extraction and gas chromatography

    NASA Technical Reports Server (NTRS)

    Merek, E. L.; Carle, G. C.

    1974-01-01

    Soil moisture content was determined by extracting soil with methanol and subsequently analyzing the extract for water by gas chromatography. With air-dried mineral soils, this method gave slightly higher moisture content values than those obtained by the oven-dry method. Moisture content was determined quantitatively in soils to which various amounts of water had been added. The complete procedure, including extraction and analysis, requires less than one hour and gives results that closely compare to the oven-dry method.

  18. Chelate-modified polymers for atmospheric gas chromatography

    NASA Technical Reports Server (NTRS)

    Christensen, W. W.; Mayer, L. A.; Woeller, F. H. (Inventor)

    1980-01-01

    Chromatographic materials were developed to serve as the stationary phase of columns used in the separation of atmospheric gases. These materials consist of a crosslinked porous polymer matrix, e.g., a divinylbenzene polymer, into which has been embedded an inorganic complexed ion such as N,N'-ethylene-bis-(acetylacetoniminato)-cobalt (2). Organic nitrogenous bases, such as pyridine, may be incorporated into the chelate polymer complexes to increase their chromatographic utility. With such materials, the process of gas chromatography is greatly simplified, especially in terms of time and quantity of material needed for a gas separation.

  19. Systematic Comparison of a Two-dimensional Ion Trap and a Three-dimensional Ion Trap Mass Spectrometer in Proteomics*S

    PubMed Central

    Mayya, Viveka; Rezaul, Karim; Cong, Yu-Sheng; Han, David

    2006-01-01

    The utility and advantages of the recently introduced two-dimensional quadrupole ion trap mass spectrometer in proteomics over the traditional three-dimensional ion trap mass spectrometer have not been systematically characterized. Here we rigorously compared the performance of these two platforms by using over 100,000 tandem mass spectra acquired with identical complex peptide mixtures and acquisition parameters. Specifically we compared four factors that are critical for a successful proteomic study: 1) the number of proteins identified, 2) sequence coverage or the number of peptides identified for every protein, 3) the data base matching SEQUEST Xcorr and Sp score, and 4) the quality of the fragment ion series of peptides. We found a 4–6-fold increase in the number of peptides and proteins identified on the two-dimensional ion trap mass spectrometer as a direct result of improvement in all the other parameters examined. Interestingly more than 70% of the doubly and triply charged peptides, but not the singly charged peptides, showed better quality of fragmentation spectra on the two-dimensional ion trap. These results highlight specific advantages of the two-dimensional ion trap over the conventional three-dimensional ion traps for protein identification in proteomic experiments. PMID:15608339

  20. IDENTIFICATION OF TRIFLURALIN METABOLITIES IN SOIL USING ION-TRAP LC/MS/MS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Trifluralin degradation in soils is complex, potentially resulting in the formation of 28 metabolites. The objective of this research was to develop an approach for the identification of trifluralin metabolites in soils using ion-trap LC/mass spectrometry (ion-trap LC/MS/MS). Authentic standards of ...

  1. Pyrolysis-high resolution gas chromatography and pyrolysis gas chromatography-mass spectrometry of kerogens and kerogen precursors

    NASA Technical Reports Server (NTRS)

    Van De Meent, D.; Brown, S. C.; Philp, R. P.; Simoneit, B. R. T.

    1980-01-01

    A series of kerogens and kerogen precursors isolated from DSDP samples, oil shales and recent algal mats have been examined by Curie point pyrolysis-high resolution gas chromatography and gas chromatography-mass spectrometry. This study has shown that the three main types of kerogens (marine, terrestrial and mixtures of both) can be characterized using these techniques. The marine (algal) kerogens yield principally aliphatic products and the terrestrial kerogens yield more aromatic and phenolic products with some n-alkanes and n-alkenes. The yields of n-alkanes and n-alkenes increase and phenols decrease with increasing geologic age, however, pyrolysis-GC cannot be used to characterize the influence of short term diagenesis on the kerogen structure.

  2. Comparison of three lychee cultivar odor profiles using gas chromatography-olfactometry and gas chromatography-sulfur detection.

    PubMed

    Mahattanatawee, Kanjana; Perez-Cacho, Pilar Ruiz; Davenport, Thomas; Rouseff, Russell

    2007-03-01

    Odor volatiles in three major lychee cultivars (Mauritius, Brewster, and Hak Ip) were examined using gas chromatography-olfactometry, gas chromatography-mass spectrometry, and gas chromatography-pulsed flame photometric detection. Fifty-nine odor-active compounds were observed including 11 peaks, which were associated with sulfur detector responses. Eight sulfur volatiles were identified as follows: hydrogen sulfide, dimethyl sulfide, diethyl disulfide, 2-acetyl-2-thiazoline, 2-methyl thiazole, 2,4-dithiopentane, dimethyl trisulfide, and methional. Mauritius contained 25% and Brewster contained 81% as much total sulfur volatiles as Hak Ip. Cultivars were evaluated using eight odor attributes: floral, honey, green/woody, tropical fruit, peach/apricot, citrus, cabbage, and garlic. Major odor differences in cabbage and garlic attributes correlated with cultivar sulfur volatile composition. The 24 odor volatiles common to all three cultivars were acetaldehyde, ethanol, ethyl-3-methylbutanoate, diethyl disulfide, 2-methyl thiazole, 1-octen-3-one, cis-rose oxide, hexanol, dimethyl trisulfide, alpha-thujone, methional, 2-ethyl hexanol, citronellal, (E)-2-nonenal, linalool, octanol, (E,Z)-2,6-nonadienal, menthol, 2-acetyl-2-thiazoline, (E,E)-2,4-nonadienal, beta-damascenone, 2-phenylethanol, beta-ionone, and 4-vinyl-guaiacol. PMID:17266328

  3. Developments of multiplexed and miniature two-dimensional quadrupole ion trap mass spectrometers

    NASA Astrophysics Data System (ADS)

    Smith, Scott A.

    Quadrupole ion trap mass spectrometry (QIT MS) is a powerful and commonly-employed method for the specific analysis of mass, composition, and structure of gas-phase ionic chemical species. Useful for a wide variety of tasks, applications of ion traps include environmental monitoring, surface analysis (including depth profiling and imaging), ion thermochemical property elucidation, protein and DNA sequencing, and high-resolution chemical separations (through ion soft-landing). Though the principles of QIT MS have been known for over half a century, innovations in instrumentation and applications continue. As new needs for specific and sensitive chemical analysis arise, so also do new and more efficient analytical devices and methods of analysis. Such a trend is exemplified through the construction of a dual-source QIT mass spectrometer (described herein) capable of multi-source chemical analyses for the purposes of enhanced proteomic sequence coverage and for the strictly-controlled comparison of the structural differences in ion populations generated by different ionization techniques. Furthermore, as mass spectrometry becomes increasingly commonplace outside the bounds of the analytical laboratory, demand for capable researcher equipment is also increasing. Advances in instrument performance, such as can be had through enhanced power efficiency and the enabling of chemical analysis of high mass-to-charge ratio (m/z) species (e.g., proteins), will open new doors to in situ chemical analysis hand-portable mass spectrometers. Hence, research into new mass analyzer designs and methods of fabrication using stereolithography apparatus (SLA) for the purpose of creating enhanced-performance mass spectrometers are accordingly described in the text of this dissertation.

  4. Determination of Vinyl Chloride at ug/l. Level in Water by Gas Chromatography

    ERIC Educational Resources Information Center

    Bellar, Thomas A.; And Others

    1976-01-01

    A quantitative method for the determination of vinyl chloride in water is presented. Vinyl chloride is transfered to the gas phase by bubbling inert gas through the water. After concentration on silica gel or Carbosieve-B, determination is by gas chromatography. Confirmation of vinyl chloride is by gas chromatography-mass spectrometry. (Author/BT)

  5. Chromatography.

    ERIC Educational Resources Information Center

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  6. Ultratrace detector for hand-held gas chromatography

    DOEpatents

    Andresen, Brian D.; Miller, Fred S.

    1999-01-01

    An ultratrace detector system for hand-held gas chromatography having high sensitivity, for example, to emissions generated during production of weapons, biological compounds, drugs, etc. The detector system is insensitive to water, air, helium, argon, oxygen, and C0.sub.2. The detector system is basically composed of a hand-held capillary gas chromatography (GC), an insulated heated redox-chamber, a detection chamber, and a vapor trap. For example, the detector system may use gas phase redox reactions and spectral absorption of mercury vapor. The gas chromatograph initially separates compounds that percolate through a bed of heated mercuric oxide (HgO) in a silica--or other metal--aerogel material which acts as an insulator. Compounds easily oxidized by HgO liberate atomic mercury that subsequently pass through a detection chamber which includes a detector cell, such as quartz, that is illuminated with a 254 nm ultra-violet (UV) mercury discharge lamp which generates the exact mercury absorption bands that are used to detect the liberated mercury atoms. Atomic mercury strongly absorbs 254 nm energy is therefore a specific signal for reducing compounds eluting from the capillary GC, whereafter the atomic mercury is trapped for example, in a silicon-aerogel trap.

  7. ANALYSIS OF HAZARDOUS WASTE AND ENVIRONMENTAL EXTRACTS BY CAPILLARY GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY AND CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    The relative sensitivities of fused-silica capillary column gas chromatography/Fourier transform infrared spectrometry (FSCC/GC/FT-IR) versus packed-column GC/FT-IR and FSCC/GC/FT-IR versus fused-silica capillary column gas chromatography/mass spectrometry (FSCC/GC/MS) were compa...

  8. Characterization of crude oils by inverse gas chromatography.

    PubMed

    Mutelet, F; Ekulu, G; Rogalski, M

    2002-09-01

    It was shown that the flocculation onset of asphaltenes in crude oils could be predicted on the basis of the inverse gas chromatography characterization of the crude oil properties. Hildebrand's solubility parameters of four crude oils were calculated from inverse chromatography data and compared with values obtained from the onset of asphaltene flocculation measurements. A good agreement was observed with three crude oils of different origin. A relation between Hildebrand's solubility parameter and linear solvation energy relationship descriptors was established and it was demonstrated that the solubility parameter of a crude oil is determined mainly with dispersion interactions and the hydrogen bond basicity. A large basicity lowers the oil solubility parameter, and increases its stability in respect to flocculation. PMID:12385392

  9. The Use of Gas Chromatography for Biogas Analysis

    NASA Astrophysics Data System (ADS)

    Andersen, Amanda; Seeley, John; Aurandt, Jennifer

    2010-04-01

    Energy from natural gas accounts for 24 percent of energy consumed in the US. Natural gas is a robust form of energy which is rich in methane content and is low in impurities. This quality suggests that it is a very clean and safe gas; it can be used in providing heat, a source for cooking, and in powering vehicles. The downside is that it is a non-renewable resource. On the contrary, methane rich gas that is produced by the breakdown of organic material in an anaerobic environment, called biogas, is a renewable energy source. This research focuses on the gas analysis portion of the creation of the anaerobic digestion and verification laboratory where content and forensic analysis of biogas is performed. Gas Chromatography is implemented as the optimal analytical tool for quantifying the components of the biogas including methane, carbon dioxide, hydrogen sulfide and siloxanes. In addition, the problems associated with the undesirable components are discussed. Anaerobic digestion of primary sludge has consistently produced about 55 percent methane; future goals of this research include studying different substrates to increase the methane yield and decrease levels of impurities in the gas.

  10. Reducing Space Charge Effects in a Linear Ion Trap by Rhombic Ion Excitation and Ejection.

    PubMed

    Zhang, Xiaohua; Wang, Yuzhuo; Hu, Lili; Guo, Dan; Fang, Xiang; Zhou, Mingfei; Xu, Wei

    2016-07-01

    Space charge effects play important roles in ion trap operations, which typically limit the ion trapping capacity, dynamic range, mass accuracy, and resolving power of a quadrupole ion trap. In this study, a rhombic ion excitation and ejection method was proposed to minimize space charge effects in a linear ion trap. Instead of applying a single dipolar AC excitation signal, two dipolar AC excitation signals with the same frequency and amplitude but 90° phase difference were applied in the x- and y-directions of the linear ion trap, respectively. As a result, mass selective excited ions would circle around the ion cloud located at the center of the ion trap, rather than go through the ion cloud. In this work, excited ions were then axially ejected and detected, but this rhombic ion excitation method could also be applied to linear ion traps with ion radial ejection capabilities. Experiments show that space charge induced mass resolution degradation and mass shift could be alleviated with this method. For the experimental conditions in this work, space charge induced mass shift could be decreased by ~50%, and the mass resolving power could be improved by ~2 times at the same time. Graphical Abstract ᅟ. PMID:27080008

  11. Reducing Space Charge Effects in a Linear Ion Trap by Rhombic Ion Excitation and Ejection

    NASA Astrophysics Data System (ADS)

    Zhang, Xiaohua; Wang, Yuzhuo; Hu, Lili; Guo, Dan; Fang, Xiang; Zhou, Mingfei; Xu, Wei

    2016-07-01

    Space charge effects play important roles in ion trap operations, which typically limit the ion trapping capacity, dynamic range, mass accuracy, and resolving power of a quadrupole ion trap. In this study, a rhombic ion excitation and ejection method was proposed to minimize space charge effects in a linear ion trap. Instead of applying a single dipolar AC excitation signal, two dipolar AC excitation signals with the same frequency and amplitude but 90° phase difference were applied in the x- and y-directions of the linear ion trap, respectively. As a result, mass selective excited ions would circle around the ion cloud located at the center of the ion trap, rather than go through the ion cloud. In this work, excited ions were then axially ejected and detected, but this rhombic ion excitation method could also be applied to linear ion traps with ion radial ejection capabilities. Experiments show that space charge induced mass resolution degradation and mass shift could be alleviated with this method. For the experimental conditions in this work, space charge induced mass shift could be decreased by ~50%, and the mass resolving power could be improved by ~2 times at the same time.

  12. Laser ablation loading of a radiofrequency ion trap

    NASA Astrophysics Data System (ADS)

    Zimmermann, K.; Okhapkin, M. V.; Herrera-Sancho, O. A.; Peik, E.

    2012-06-01

    The production of ions via laser ablation for the loading of radiofrequency (RF) ion traps is investigated using a nitrogen laser with a maximum pulse energy of 0.17 mJ and a peak intensity of about 250 MW/cm2. A time-of-flight mass spectrometer is used to measure the ion yield and the distribution of the charge states. Singly charged ions of elements that are presently considered for the use in optical clocks or quantum logic applications could be produced from metallic samples at a rate of the order of magnitude 105 ions per pulse. A linear Paul trap was loaded with Th+ ions produced by laser ablation. An overall ion production and trapping efficiency of 10-7 to 10-6 was attained. For ions injected individually, a dependence of the capture probability on the phase of the RF field has been predicted. In the experiment this was not observed, presumably because of collective effects within the ablation plume.

  13. Development of a quadrupole ion trap mass spectrometer

    NASA Astrophysics Data System (ADS)

    Hebert, Joseph Ellis

    Because of its potential to be made portable the quadrupole ion trap (QPIT) is a prime candidate for specialized applications such as atmospheric studies, other field measurements, or measurements anywhere a laboratory instrument would be prohibitively inconvenient. To utilize the QPIT in such ways it is necessary to design and construct custom built instruments. A QPIT mass spectrometer was constructed as the foundation for such future development. Two ionization schemes were employed. Direct electron bombardment was used for in situ ion production, and UV photoionization was used to produce ions external to the trap. Calibration measurements determined that the system performed as theory dictated. It was also demonstrated that the system was capable of sampling the atmosphere and detecting the presence of an atmospheric contaminant. Finally, DC bias foils were invented as a novel approach to mass isolation in the trap. The use of DC bias foils was demonstrated to be an exceptionally easy and inexpensive method of controlling the contents of the QPIT.

  14. Upgrade of the electron beam ion trap in Shanghai

    NASA Astrophysics Data System (ADS)

    Lu, D.; Yang, Y.; Xiao, J.; Shen, Y.; Fu, Y.; Wei, B.; Yao, K.; Hutton, R.; Zou, Y.

    2014-09-01

    Over the last few years the Shanghai electron beam ion trap (EBIT) has been successfully redesigned and rebuilt. The original machine, developed under collaboration with the Shanghai Institute of Applied Physics, first produced an electron beam in 2005. It could be tuned with electron energies between 1 and 130 keV and beam current up to 160 mA. After several years of operation, it was found that several modifications for improvements were necessary to reach the goals of better electron optics, higher photon detection, and ion injection efficiencies, and more economical running costs. The upgraded Shanghai-EBIT is made almost entirely from Ti instead of stainless steel and achieves a vacuum of less than 10-10 Torr, which helps to minimize the loss of highly changed ions through charge exchange. Meanwhile, a more compact structure and efficient cryogenic system, and excellent optical alignment have been of satisfactory. The magnetic field in the central trap region can reach up till 4.8 T with a uniformity of 2.77 × 10-4. So far the upgraded Shanghai-EBIT has been operated up to an electron energy of 151 keV and a beam current of up to 218 mA, although promotion to even higher energy is still in progress. Radiation from ions as highly charged as Xe53+, 54+ has been produced and the characterization of current density is estimated from the measured electron beam width.

  15. Upgrade of the electron beam ion trap in Shanghai

    SciTech Connect

    Lu, D.; Yang, Y.; Xiao, J.; Shen, Y.; Fu, Y.; Wei, B.; Yao, K.; Hutton, R.; Zou, Y.

    2014-09-15

    Over the last few years the Shanghai electron beam ion trap (EBIT) has been successfully redesigned and rebuilt. The original machine, developed under collaboration with the Shanghai Institute of Applied Physics, first produced an electron beam in 2005. It could be tuned with electron energies between 1 and 130 keV and beam current up to 160 mA. After several years of operation, it was found that several modifications for improvements were necessary to reach the goals of better electron optics, higher photon detection, and ion injection efficiencies, and more economical running costs. The upgraded Shanghai-EBIT is made almost entirely from Ti instead of stainless steel and achieves a vacuum of less than 10{sup −10} Torr, which helps to minimize the loss of highly changed ions through charge exchange. Meanwhile, a more compact structure and efficient cryogenic system, and excellent optical alignment have been of satisfactory. The magnetic field in the central trap region can reach up till 4.8 T with a uniformity of 2.77 × 10{sup −4}. So far the upgraded Shanghai-EBIT has been operated up to an electron energy of 151 keV and a beam current of up to 218 mA, although promotion to even higher energy is still in progress. Radiation from ions as highly charged as Xe{sup 53+,} {sup 54+} has been produced and the characterization of current density is estimated from the measured electron beam width.

  16. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-07-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal for instructional use, especially to illustrate HS analysis or as an alternative to solid-phase microextraction (SPME) to which it is very similar. The basic principles and practice of HS-GC using SDME are described, including a complete review of the literature. Some possible experiments are suggested using water and N -methylpyrrolidone (NMP) as solvents.

  17. Gas-liquid chromatography in lunar organic analysis.

    NASA Technical Reports Server (NTRS)

    Gehrke, C. W.

    1972-01-01

    Gas-liquid chromatography (GLC) is a powerful and sensitive method for the separation and detection of organic compounds at nanogram levels. The primary requirement for successful analyses is that the compounds of interest must be volatile under the chromatographic conditions employed. Nonvolatile organic compounds must be converted to volatile derivatives prior to analysis. The derivatives of choice must be both amenable to chromatographic separation and be relatively stable. The condition of volatility necessitates the development of efficient derivatization reactions for important groups of compounds as amino acids, carbohydrates, nucleosides, etc. Trimethylsilylation and trifluoroacetylation represent specific areas of recent prominence. Some relevant practical aspects of GLC are discussed.

  18. [Determination of acetochlor and oxyfluorfen by capillary gas chromatography].

    PubMed

    Xiang, Wen-Sheng; Wang, Xiang-Jing; Wang, Jing; Wang, Qing

    2002-09-01

    A method is described for the determination of acetochlor and oxyfluorfen by capillary gas chromatography with FID and an SE-30 capillary column (60 m x 0.53 mm i. d., 1.5 microm), using dibutyl phthalate as the internal standard. The standard deviations for acetochlor and oxyfluorfen concentration(mass fraction) were 0.44% and 0.47% respectively. The relative standard deviations for acetochlor and oxyfluorfen were 0.79% and 0.88% and the average recoveries for acetochlor and oxyfluorfen were 99.3% and 101.1% respectively. The method is simple, rapid and accurate. PMID:16358708

  19. Capillary gas chromatography with two new moderately high temperature phases.

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.

    1972-01-01

    Gas chromatography test results are presented for two new moderately high-temperature phases of Dexsil 400-GC with free hydroxyl end groups (uncapped) and with end groups covered by trimethyl silyl groups (capped). The two Dexsil 400-GC phases were tested for their ability to resolve N-TFA-DL-(+)-2-butyl esters and n-butyl esters, as well as fatty acid methyl esters and hydrocarbon standards. Generally the more polar uncapped phase was superior to the capped phase in all separation comparisons, except for the hydrocarbons.

  20. Thermal History Of PMRs Via Pyrolysis-Gas Chromatography

    NASA Technical Reports Server (NTRS)

    Gluyas, Richard E.; Alston, William B.; Snyder, William J.

    1994-01-01

    Pyrolysis-gas chromatography (PY-GC) useful as analytical technique to determine extents of cure or postcure of PMR-15 polyimides and to lesser extent, cumulative thermal histories of PMR-15 polyimides exposed to high temperatures. Also applicable for same purposes to other PMR polyimides and to composite materials containing PMR polyimides. Valuable in reducing costs and promoting safety in aircraft industry by helping to identify improperly cured or postcured PMR-15 composite engine and airframe components and helping to identify composite parts nearing ends of their useful lives.

  1. Continuous monitoring of a changing sample by multiplex gas chromatography

    NASA Technical Reports Server (NTRS)

    Valentin, Jose R.; Hall, Kirsten W.; Becker, Joseph F.

    1990-01-01

    Results are presented from a study in which a continuously changed gaseous sample was monitored by multiplex gas chromatography (MGC), using the exponential dilution (ED) technique of Ritter and Adams (1976) to change the composition and concentration of a gaseous mixture in such a way as to imitate changes in the atmospheric gases sampled by a descending aircraft. A calibration of the MGC system was performed with four different rates of sample dilution, and the errors resulting from various degrees of change in the sample concentration were determined.

  2. An electrodynamic ion funnel interface for greater sensitivity and higher throughput with linear ion trap mass spectrometers

    NASA Astrophysics Data System (ADS)

    Page, Jason S.; Tang, Keqi; Smith, Richard D.

    2007-09-01

    An electrospray ionization interface incorporating an electrodynamic ion funnel has been designed and implemented on a linear ion trap mass spectrometer (Thermo Electron, LTQ). We found ion transmission to be greatly improved by replacing the standard capillary-skimmer interface with the capillary-ion funnel interface. An infusion study using a serial dilution of a reserpine solution showed that ion injection (accumulation) times to fill the ion trap at a given automatic gain control (AGC) target value were reduced by ~90% which resulted in an ~10-fold increase in peak intensities. In liquid chromatography tandem MS (LC-MS/MS) experiments performed using a global protein digest sample from the bacterium, Shewanella oneidensis, more peptides and proteins were identified when the ion funnel interface was used in place of the standard interface. This improvement was most pronounced at lower sample concentrations, where extended ion accumulation times are required, resulting in an ~2-fold increase in the number of protein identifications. Implementation of the ion funnel interface on a LTQ Fourier transform (FT) mass spectrometer showed a ~25-50% reduction in spectrum acquisition time. The duty cycle improvement in this case was due to the ion accumulation event contributing a larger portion to the total spectrum acquisition time.

  3. An electrodynamic ion funnel interface for greater sensitivity and higher throughput with linear ion trap mass spectrometers

    SciTech Connect

    Page, Jason S.; Tang, Keqi; Smith, Richard D.

    2007-09-01

    An electrospray ionization interface incorporating an electrodynamic ion funnel has been designed and implemented in conjunction with a linear ion trap mass spectrometer (Thermo Electron, LTQ). We found ion transmission to be greatly improved by replacing the standard capillary-skimmer interface with the capillary-ion funnel interface. An infusion study using a serial dilution of a reserpine solution showed that ion injection times to fill the ion trap were reduced by ~90% which resulted in an ~10-fold increase in reported peak intensities. In liquid chromatography (LC)-MS and LC tandem MS (MS/MS) experiments performed using a proteomic sample from the bacterium, Shewanella oneidensis, the ion funnel interface provided an ~7-fold reduction in ion injection (accumulation) times. In a series of LC-MS/MS experiments we found that more dilute S. oneidensis samples provided more peptide and protein identifications when the ion funnel interface was used in place of the standard interface. This improvement was most pronounced at lower sample concentrations, where extended ion accumulation times are required, resulting in an ~2-fold increase in the number of protein identifications. Implementation of the ion funnel interface with a LTQ Fourier transform (FT) MS requiring much greater ion populations resulted in spectrum acquisition times reduced by ~25 to 50%.

  4. Assessment of the ion-trap mass spectrometer for routine qualitative and quantitative analysis of drugs of abuse extracted from urine.

    PubMed

    Vorce, S P; Sklerov, J H; Kalasinsky, K S

    2000-10-01

    The ion-trap mass spectrometer (MS) has been available as a detector for gas chromatography (GC) for nearly two decades. However, it still occupies a minor role in forensic toxicology drug-testing laboratories. Quadrupole MS instruments make up the majority of GC detectors used in drug confirmation. This work addresses the use of these two MS detectors, comparing the ion ratio precision and quantitative accuracy for the analysis of different classes of abused drugs extracted from urine. Urine specimens were prepared at five concentrations each for amphetamine (AMP), methamphetamine (METH), benzoylecgonine (BZE), delta9-carboxy-tetrahydrocannabinol (delta9-THCCOOH), phencyclidine (PCP), morphine (MOR), codeine (COD), and 6-acetylmorphine (6-AM). Concentration ranges for AMP, METH, BZE, delta9-THCCOOH, PCP, MOR, COD, and 6-AM were 50-2500, 50-5000, 15-800, 1.5-65, 1-250, 500-32000, 250-21000, and 1.5-118 ng/mL, respectively. Sample extracts were injected into a GC-quadrupole MS operating in selected ion monitoring (SIM) mode and a GC-ion-trap MS operating in either selected ion storage (SIS) or full scan (FS) mode. Precision was assessed by the evaluation of five ion ratios for n = 15 injections at each concentration using a single-point calibration. Precision measurements for SIM ion ratios provided coefficients of variation (CV) between 2.6 and 9.8% for all drugs. By comparison, the SIS and FS data yielded CV ranges of 4.0-12.8% and 4.0-11.2%, respectively. The total ion ratio failure rates were 0.2% (SIM), 0.7% (SIS), and 1.2% (FS) for the eight drugs analyzed. Overall, the SIS mode produced stable, comparable mean ratios over the concentration ranges examined, but had greater variance within batch runs. Examination of postmortem and quality-control samples produced forensically accurate quantitation by SIS when compared to SIM. Furthermore, sensitivity of FS was equivalent to SIM for all compounds examined except for 6-AM. PMID:11043665

  5. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid... pressure. The device may include accessories such as columns, gases, column supports, and liquid...

  6. High performance mini-gas chromatography-flame ionization detector system based on micro gas chromatography column

    NASA Astrophysics Data System (ADS)

    Zhu, Xiaofeng; Sun, Jianhai; Ning, Zhanwu; Zhang, Yanni; Liu, Jinhua

    2016-04-01

    Monitoring Volatile organic compounds (VOCs) was a very important measure for preventing environmental pollution, therefore, a mini gas chromatography (GC) flame ionization detector (FID) system integrated with a mini H2 generator and a micro GC column was developed for environmental VOC monitoring. In addition, the mini H2 generator was able to make the system explode from far away due to the abandoned use of a high pressure H2 source. The experimental result indicates that the fabricated mini GC FID system demonstrated high repeatability and very good linear response, and was able to rapidly monitor complicated environmental VOC samples.

  7. High performance mini-gas chromatography-flame ionization detector system based on micro gas chromatography column.

    PubMed

    Zhu, Xiaofeng; Sun, Jianhai; Ning, Zhanwu; Zhang, Yanni; Liu, Jinhua

    2016-04-01

    Monitoring Volatile organic compounds (VOCs) was a very important measure for preventing environmental pollution, therefore, a mini gas chromatography (GC) flame ionization detector (FID) system integrated with a mini H2 generator and a micro GC column was developed for environmental VOC monitoring. In addition, the mini H2 generator was able to make the system explode from far away due to the abandoned use of a high pressure H2 source. The experimental result indicates that the fabricated mini GC FID system demonstrated high repeatability and very good linear response, and was able to rapidly monitor complicated environmental VOC samples. PMID:27131686

  8. Novel stationary phases based on asphaltenes for gas chromatography.

    PubMed

    Boczkaj, Grzegorz; Momotko, Malwina; Chruszczyk, Dorota; Przyjazny, Andrzej; Kamiński, Marian

    2016-07-01

    We present the results of investigations on the possibility of the application of the asphaltene fraction isolated from the oxidized residue from vacuum distillation of crude oil as a stationary phase for gas chromatography. The results of the investigation revealed that the asphaltene stationary phases can find use for the separation of a wide range of volatile organic compounds. The experimental values of Rohrschneider/McReynolds constants characterize the asphaltenes as stationary phases of medium polarity and selectivity similar to commercially available phases based on alkyl phthalates. Isolation of asphaltenes from the material obtained under controlled process conditions allows the production of a stationary phase having reproducible sorption properties and chromatographic columns having the same selectivity. Unique selectivity and high thermal stability make asphaltenes attractive as a material for stationary phases for gas chromatography. A low production cost from a readily available raw material (oxidized petroleum bitumens) is an important economic factor in case of application of the asphaltene stationary phases for preparative and process separations. PMID:27144876

  9. Quantification of 2-acetyl-1-pyrroline in rice by stable isotope dilution assay through headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry.

    PubMed

    Maraval, Isabelle; Sen, Kemal; Agrebi, Abdelhamid; Menut, Chantal; Morere, Alain; Boulanger, Renaud; Gay, Frédéric; Mestres, Christian; Gunata, Ziya

    2010-08-24

    A new and convenient synthesis of 2-acetyl-1-pyrroline (2AP), a potent flavor compound in rice, and its ring-deuterated analog, 2-acetyl-1-d(2)-pyrroline (2AP-d(2)), was reported. A stable isotope dilution assay (SIDA), involving headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-positive chemical ionization-ion trap-tandem mass spectrometry (GC-PCI-IT-MS-MS), was developed for 2AP quantification. A divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used for HS-SPME procedure and parameters affecting analytes recovery, such as extraction time and temperature, pH and salt, were studied. The repeatability of the method (n=10) expressed as relative standard deviation (RSD) was 11.6%. A good linearity was observed from 5.9 to 779 ng of 2AP (r(2)=0.9989). Limits of detection (LOD) and quantification (LOQ) for 2AP were 0.1 and 0.4 ng g(-1) of rice, respectively. The recovery of spiked 2AP from rice matrix was almost complete. The developed method was applied to the quantification of 2AP in aerial parts and grains of scented and non-scented rice cultivars. PMID:20800726

  10. Quantification of prominent volatile compounds responsible for muskmelon and watermelon aroma by purge and trap extraction followed by gas chromatography-mass spectrometry determination.

    PubMed

    Fredes, Alejandro; Sales, Carlos; Barreda, Mercedes; Valcárcel, Mercedes; Roselló, Salvador; Beltrán, Joaquim

    2016-01-01

    A dynamic headspace purge-and-trap (DHS-P&T) methodology for the determination and quantification of 61 volatile compounds responsible for muskmelon and watermelon aroma has been developed and validated. The methodology is based on the application of purge-and-trap extraction followed by gas chromatography coupled to (ion trap) mass spectrometry detection. For this purpose two different P&T sorbent cartridges have been evaluated. The influence of different extraction factors (sample weight, extraction time, and purge flow) on extraction efficiency has been studied and optimised using response surface methodology. Precision, expressed as repeatability, has been evaluated by analysing six replicates of real samples, showing relative standard deviations between 3% and 27%. Linearity has been studied in the range of 10-6130 ng mL(-1) depending on the compound response, showing coefficients of correlation between 0.995 and 0.999. Detection limits ranged between 0.1 and 274 ng g(-1). The methodology developed is well suited for analysis of large numbers of muskmelon and watermelon samples in plant breeding programs. PMID:26213027

  11. Rapid determination of alkylphenols in aqueous samples by in situ acetylation and microwave-assisted headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry.

    PubMed

    Wu, Yu-Pei; Wang, Yu-Chen; Ding, Wang-Hsien

    2012-08-01

    A rapid and solvent-free procedure for the determination of 4-tert-octylphenol and 4-nonylphenol isomers in aqueous samples is described. The method involves in-situ acetylation and microwave-assisted headspace solid-phase microextraction prior to their determination using gas chromatography-ion trap mass spectrometry operated in the selected ion storage mode. The dual experimental protocols to evaluate the effects of various derivatization and extraction parameters were investigated and the conditions optimized. Under optimized conditions, 300 μL of acetic anhydride mixed with 1 g of potassium hydrogencarbonate and 2 g of sodium chloride in a 20 mL aqueous sample were efficiently extracted by a 65 μm polydimethylsiloxane-divinylbenzene fiber that was located in the headspace when the system was microwave irradiated at 80 W for 5 min. The limits of quantitation were 5 and 50 ng/L for 4-tert-octylphenol and 4-nonylphenol isomers, respectively. The precision for these analytes, as indicated by relative standard deviations, were less than 8% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 to 88%. A standard addition method was used to quantitate 4-tert-octylphenol and 4-nonylphenol isomers, and the concentrations ranged from 120 to 930 ng/L in various environmental water samples. PMID:22899640

  12. Identification of polychlorinated styrene compounds in heron tissues by gas-liquid chromatography-mass spectrometry

    USGS Publications Warehouse

    Reichel, W.L.; Prouty, R.M.; Gay, M.L.

    1977-01-01

    Unknown compounds detected in Ardea herodias tissues are identified by gas-liquid chromatography-mass spectrometry as residues of octachlorostyrene. Heptachlorostyrene and hexachlorostyrene were tentatively identified.

  13. Laboratory Astrophysics Using the Electron Beam Ion Trap

    NASA Astrophysics Data System (ADS)

    Brown, Gregory V.

    2014-06-01

    X-ray astronomy has seen profound growth in discovery space for over a decade resulting almost entirely from the successful operation of three X-ray observatories: Chandra, XMM-Newton, and Suzaku. The high sensitivity, high resolution instrumentation on these satellites have provided the X-ray astrophysicists with relatively straightforward access to powerful line diagnostics that tightly constrain the physical parameters of celestial sources. For example, accurate measurements of transition energies, line shapes, and intensities provide quantitative measures of a velocity fields, electron densities and temperatures. X-ray measurements probe sources unattainable by any other wavelength bands, such as the regions of accretion disks near black holes, and the hot intracluster medium in clusters of galaxies. Thus, X-ray astronomy in the age of Chandra, XMM-Newton, and Suzaku provides important pieces of the puzzles necessary to understand the formation and evolution of galaxies, stars, the phenomena near black holes, and the evolution of the universe as a whole. Unfortunately, accurate unambiguous interpretation of high quality spectra is often limited by the accuracy and completeness of atomic data rather than the uncertainties related to counting statistics or instrumentation. Starting over twenty years ago, the electron beam ion trap facility at Lawrence Livermore National Laboratory has been used to benchmark spectral models used to interpret celestial data, and to address specific problems facing the astrophysics community. More recently, the portable FLASH-EBIT, built and maintained at the Max Planck Institute for Nuclear Physics, Heidelberg and coupled to third and fourth generation light sources has opened new measurement regimes relavant to the high energy astrophysics community. Selected results will be presented. This work performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344

  14. Eliminating degradation and uncovering ion-trapping dynamics in electrochromic WO3 thin films

    NASA Astrophysics Data System (ADS)

    Wen, Rui-Tao; Granqvist, Claes G.; Niklasson, Gunnar A.

    2015-10-01

    There is keen interest in the use of amorphous WO3 thin films as cathodic electrodes in transmittance-modulating electrochromic devices. However, these films suffer from ion-trapping-induced degradation of optical modulation and reversibility on extended Li+-ion exchange. Here, we demonstrate that ion-trapping-induced degradation, which is commonly believed to be irreversible, can be successfully eliminated by constant-current-driven de-trapping; that is, WO3 films can be rejuvenated and regain their initial highly reversible electrochromic performance. Pronounced ion trapping occurs when x exceeds ~0.65 in LixWO3 during ion insertion. We find two main kinds of Li+-ion-trapping site (intermediate and deep) in WO3, where the intermediate ones are most prevalent. Li+ ions can be completely removed from intermediate traps but are irreversibly bound in deep traps. Our results provide a general framework for developing and designing superior electrochromic materials and devices.

  15. Eliminating degradation and uncovering ion-trapping dynamics in electrochromic WO3 thin films

    PubMed Central

    Wen, Rui-Tao; Granqvist, Claes G.; Niklasson, Gunnar A.

    2015-01-01

    Amorphous WO3 thin films are of keen interest as cathodic electrodes in transmittance-modulating electrochromic devices. However, these films suffer from ion-trapping-induced degradation of optical modulation and reversibility upon extended Li+-ion exchange. Here, we demonstrate that ion-trapping-induced degradation, which is commonly believed to be irreversible, can be successfully eliminated by constant-current-driven de-trapping, i.e., WO3 films can be rejuvenated and regain their initial highly reversible electrochromic performance. Pronounced ion-trapping occurs when x exceeds ~0.65 in LixWO3 during ion insertion. We find two main kinds of Li+-ion trapping sites (intermediate and deep) in WO3, where the intermediate ones are most prevalent. Li+-ions can be completely removed from intermediate traps but are irreversibly bound in deep traps. Our results provide a general framework for developing and designing superior electrochromic materials and devices. PMID:26259104

  16. in situ plasma removal of surface contaminants from ion trap electrodes

    SciTech Connect

    Haltli, Raymond A.

    2015-04-01

    This research resulted in a construction and implementation of an in situ plasma discharge to remove surface contaminants from electrodes in an ion trapping experimental system is presented with results.

  17. Guidelines for Designing Surface Ion Traps Using the Boundary Element Method.

    PubMed

    Hong, Seokjun; Lee, Minjae; Cheon, Hongjin; Kim, Taehyun; Cho, Dong-Il Dan

    2016-01-01

    Ion traps can provide both physical implementation of quantum information processing and direct observation of quantum systems. Recently, surface ion traps have been developed using microfabrication technologies and are considered to be a promising platform for scalable quantum devices. This paper presents detailed guidelines for designing the electrodes of surface ion traps. First, we define and explain the key specifications including trap depth, q-parameter, secular frequency, and ion height. Then, we present a numerical-simulation-based design procedure, which involves determining the basic assumptions, determining the shape and size of the chip, designing the dimensions of the radio frequency (RF) electrode, and analyzing the direct current (DC) control voltages. As an example of this design procedure, we present a case study with tutorial-like explanations. The proposed design procedure can provide a practical guideline for designing the electrodes of surface ion traps. PMID:27136559

  18. Guidelines for Designing Surface Ion Traps Using the Boundary Element Method

    PubMed Central

    Hong, Seokjun; Lee, Minjae; Cheon, Hongjin; Kim, Taehyun; Cho, Dong-il “Dan”

    2016-01-01

    Ion traps can provide both physical implementation of quantum information processing and direct observation of quantum systems. Recently, surface ion traps have been developed using microfabrication technologies and are considered to be a promising platform for scalable quantum devices. This paper presents detailed guidelines for designing the electrodes of surface ion traps. First, we define and explain the key specifications including trap depth, q-parameter, secular frequency, and ion height. Then, we present a numerical-simulation-based design procedure, which involves determining the basic assumptions, determining the shape and size of the chip, designing the dimensions of the radio frequency (RF) electrode, and analyzing the direct current (DC) control voltages. As an example of this design procedure, we present a case study with tutorial-like explanations. The proposed design procedure can provide a practical guideline for designing the electrodes of surface ion traps. PMID:27136559

  19. Felion: a Cryogenic Ion Trap Apparatus for Spectroscopic Studies with Felix

    NASA Astrophysics Data System (ADS)

    Brunken, S.; Kluge, L.; Fanghanel, S.; Potapov, A.; Asvany, O.; Schlemmer, S.; Oomens, J.; Redlich, B.; Stoffels, A.

    2013-06-01

    The combination of ion trapping techniques with sensitive action spectroscopy schemes has been developed in recent years as a powerful tool to obtain spectra of gas-phase molecular ions from the UV to the (F)IR spectral regions. Here we report on the status of a specifically designed, dedicated cryogenic 22-pole ion trap apparatus (FELion), developed and built in Cologne, Germany, and intended to be installed permanently at the "Free-Electron Lasers for Infrared eXperiments" (FELIX) facility in Nijmegen, the Netherlands. This instrument will allow to record gas-phase IR and FIR spectra of mass-selected, internally cold molecular ions at temperatures in the range 4-300 K. By the use of diverse ionization methods, e.g. electron impact and electrospray ionization, a multitude of molecular ions can be generated and stored in the trap, including astrophysically relevant species ranging in size from the three-atomic H_3^+ up to large polycyclic aromatic hydrocarbon (PAH) ions, but also biomolecular ions like amino acids, peptides, or nucleobases. In combination with the powerful (F)IR radiation of the free electron lasers FELIX-1 and -2 (60-2500 cm^{-1}) and FLARE (6-100 cm^{-1}) at the FELIX facility, a variety of action spectroscopy schemes can be employed to study the ro-vibrational spectra of the stored ions, such as IR multiphoton dissociation, (F)IR/UV double resonance spectroscopy, or the method of laser induced reactions (LIR). In this talk we will give a detailed account of the experimental setup and present the first results obtained with the new apparatus. e.g., S. Schlemmer, E. Lescop, J. von Richthofen, D. Gerlich, and M. A. Smith, J. Chem. Phys. 117, 2068 (2002) J. Oomens, B. G. Sartakov, G. Meijer, and G. van Helden, Int. J. Mass Spectrom. 254, 1 (2006) T. R. Rizzo, J. A. Stearns, and O. V. Boyarkin, International Reviews in Physical Chemistry 28, 481 (2009) FLARE: Free-electron Laser for Advanced spectroscopy and high-Resolution Experiments

  20. Laser-based studies with an ion-trap mass spectrometer: Ion tomography and analytical applications

    NASA Astrophysics Data System (ADS)

    Alexander, M. L.; Cisper, M. E.; Hemberger, P. H.; Nogar, N. S.; Williams, J. D.; Syka, J. E. P.

    The iron trap mass spectrometer (ITMS) is an ion storage device which consists of two hyperbolic endcaps and a hyperbolic ring electrode. This forms a trapping cavity having a volume of several cm(sup 3). An RF potential applied to the ring electrode produces a time-varying potential which can be used to trap and/or manipulate ions under controlled conditions. This device has been used in ion trapping studies for a number of years. More recently, a commercial version has been produced and sold which allows for mass-selective ejection of trapped ions, with subsequent detection by an electron multiplier. In this mode, it operates as a compact, high efficiency, high resolution mass spectrometer. The instrument has found applications in GC/MS, in tandem mass spectroscopy and in portable mass spectral analysis. In this manuscript, we present a survey of recent results incorporating laser desorption, ionization, or photodissociation with ITMS. In one instance, we describe the use of laser photodissociation to map the spatial distribution of trapped ions in the ITMS. In this tomographic study, we have parameterized the effects of trapping potential, buffer gas pressure, supplementary RF-potential, and laser intensity. In separate studies, laser desorption was used to generate gas phase ions in the ITMS from a solid probe, by irradiation of both neat and matrix-dissolved samples. The latter experiment produced both high molecular weight ions and significant numbers of negative ions.

  1. 'Programming' Electron Beam Ion Traps To Produce Atomic Data Relevant To Plasma Physics

    SciTech Connect

    Currell, Fred; O'Rourke, Brian; Kavanagh, Anthony; Li Yueming; Nakamura, Nobuyuki; Ohtani, Shunsuke; Watanabe, Hirofumi

    2009-09-10

    After a brief review of the processes taking place in electron beam ions traps (EBITs), the means by which EBITs are used to make measurements of electron impact ionization cross-sections and dielectronic recombination resonance strengths are discussed. In particular, results from a study involving holmium ions extracted from an electron beam ion trap are used to illustrate a technique for studying dielectronic recombination in open-shell target ions.

  2. In situ plasma removal of surface contaminants from ion trap electrodes

    SciTech Connect

    Haltli, Raymond A.

    2015-05-01

    In this thesis, the construction and implementation of an in situ plasma discharge designed to remove surface contaminants from electrodes in an ion trapping experimental system is presented with results. In recent years, many advances have been made in using ion traps for quantum information processing. All of the criteria defined by DiVincenzo for using ion traps for implementing a quantum computer have been individually demonstrated, and in particular surface traps provide a scalable platform for ions. In order to be used for quantum algorithms, trapped ions need to be cooled to their motional (quantum mechanical) ground state. One of the hurdles in integrating surface ion traps for a quantum computer is minimizing electric field noise, which causes the ion to heat out of its motional ground state and which increases with smaller ion-to-electrode distances realized with surface traps. Surface contamination of trap electrodes is speculated to be the primary source of electric field noise. The main goal achieved by this work was to implement an in situ surface cleaning solution for surface electrode ion traps, which would not modify the ion trap electrode surface metal. Care was taken in applying the RF power in order to localize a plasma near the trap electrodes. A method for characterizing the energy of the plasma ions arriving at the ion trap surface is presented and results for plasma ion energies are shown. Finally, a method for quantifying the effectiveness of plasma cleaning of trap electrodes, using the surface analysis technique of X-ray photoelectron spectroscopy for measuring the amount and kind of surface contaminants, is described. A significant advantage of the trap electrode surface cleaning method presented here is the minimal changes necessary for implementation on a working ion trap experimental system.

  3. Applications of Hadamard transform to gas chromatography/mass spectrometry and liquid chromatography/mass spectrometry.

    PubMed

    Lin, Cheng-Huang; Kaneta, Takashi; Chen, Hung-Ming; Chen, Wen-Xiong; Chang, Hung-Wei; Liu, Ju-Tsung

    2008-08-01

    Successful application of the Hadamard transform (HT) technique to gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS) is described. Novel sample injection devices were developed to achieve multiple sample injections in both GC and LC instruments. Air pressure was controlled by an electromagnetic valve in GC, while a syringe pump and Tee connector were employed for the injection device in LC. Two well-known, abused drugs, 3,4-methylenedioxy-N-methylamphetamine (MDMA) and N, N-dimethyltryptamine (DMT), were employed as model samples. Both of the injection devices permitted precise successive injections, resulting in clearly modulated chromatograms encoded by Hadamard matrices. After inverse Hadamard transformation of the encoded chromatogram, the signal-to-noise (S/N) ratios of the signals were substantially improved compared with those expected from theoretical values. The S/N ratios were enhanced approximately 10-fold in HT-GC/MS and 6.8 in HT-LC/MS, using the matrices of 1023 and 511, respectively. The HT-GC/MS was successfully applied to the determination of MDMA in the urine sample of a suspect. PMID:18570388

  4. Gas chromatography flow rates for determining deuterium/hydrogen ratios of natural gas by gas chromatography/high-temperature conversion/isotope ratio mass spectrometry.

    PubMed

    Jia, Wanglu; Peng, Ping'an; Liu, Jinzhong

    2008-08-01

    The effects of the gas chromatography flow rate on the determination of the deuterium/hydrogen (D/H) ratios of natural gas utilising gas chromatography/high-temperature conversion/isotope ratio mass spectrometry (GC/TC/IRMS) have been evaluated. In general, the measured deltaD values of methane, ethane and propane decrease with increase in column flow rate. When the column flow rate is 1 mL/min or higher, which is commonly used for the determination of D/H ratios of natural gas, the organic H in gas compounds may not be completely converted into hydrogen gas. Based on the results of experiments conducted on a GC column with an i.d. of 0.32 mm, a GC flow rate of 0.6 mL/min is proposed for determining the D/H ratios of natural gas by GC/TC/IRMS. Although this value may be dependent on the instrument conditions used in this work, we believe that correct deltaD values of organic compounds with a few carbon atoms are obtained only when relatively low GC flow rates are used for D/H analysis by GC/TC/IRMS. Moreover, as the presence of trace water could significantly affect the determination of D/H ratios, a newly designed inlet liner was used to remove trace water contained in some gas samples. PMID:18636428

  5. Identification of New Metabolites of Bacterial Transformation of Indole by Gas Chromatography-Mass Spectrometry and High Performance Liquid Chromatography

    PubMed Central

    Arora, Pankaj Kumar

    2014-01-01

    Arthrobacter sp. SPG transformed indole completely in the presence of an additional carbon source. High performance liquid chromatography and gas chromatography-mass spectrometry detected indole-3-acetic acid, indole-3-glyoxylic acid, and indole-3-aldehyde as biotransformation products. This is the first report of the formation of indole-3-acetic acid, indole-3-glyoxylic acid, and indole-3-aldehyde from indole by any bacterium. PMID:25548566

  6. Low thermal mass gas chromatography: principles and applications.

    PubMed

    Luong, Jim; Gras, Ronda; Mustacich, Robert; Cortes, Hernan

    2006-01-01

    In gas chromatography (GC), temperature programming is often considered to be the second most important parameter to control, the first being column selectivity. A radically new GC technology to achieve ultrafast temperature programming with an unprecedented cool down time and low power consumption has recently become available. This technology is referred to as low thermal mass GC (LTMGC). Though the technology has its roots in resistive heating, which forms the basis of principle and design concept, the approach taken to achieve ultrafast heating and cool down time by LTMGC represents a significant break-through in GC. Despite some rectifiable shortcomings, LTMGC has proven to be an ideal methodology to deliver near/real time GC data, high precision, and high throughput applications. It is a new approach for modern high-speed GC. This paper documents the fundamental design principles behind LTMGC, performance data, and examples of applications investigated. PMID:16774710

  7. Design, testing, and simulation of microscale gas chromatography columns

    SciTech Connect

    Hudson, M.L.; Kottenstette, R.; Matzke, C.M.; Frye-Mason, G.C.; Shollenberger, K.A.; Adkins, D.R.; Wong, C.C.

    1998-08-01

    A microscale gas chromatography column is one component in a microscale chemistry laboratory for detecting chemical agents. Several columns were fabricated using the Bosch etch process which allows deep, high aspect ratio channels of rectangular cross-section. A design tool, based on analytical models, was developed to evaluate the effects of operating conditions and column specifications on separation resolution and time. The effects of slip flow, channel configuration, and cross-sectional shape were included to evaluate the differences between conventional round, straight columns and the microscale rectangular, spiral columns. Experimental data were obtained and compared with the predicted flowrates and theoretical number of plates. The design tool was then employed to select more optimum channel dimensions and operating conditions for high resolution separations.

  8. Field gas chromatography-mass spectrometry for fast analysis.

    PubMed

    Makas, Alexei L; Troshkov, Mikhail L

    2004-02-01

    The objective of this presentation is to demonstrate the original device and procedure for fast gas chromatography-mass spectrometry (GC-MS) analysis of gaseous and liquid samples and to discuss its features and capabilities. The concept was developed in order to expand the range of compounds suitable for GC separation and to reduce the time of analysis. Field GC-MS, consisting of original "concentrator-thermodesorber" (CTD) unit, multiple module GC system and compact magnetic mass spectrometer with powerful two-stage vacuum system and multicollector ion detector, is represented. The whole weight of the device is 90 kg. Power consumption is 250 W. The device and analytical procedures allow high speed screening of toxic substances in air and extracts within 100 s per sample. The examples of applications are described, including fast screening of tributyl phosphate (TBP) in air at low ppt level at the rate 1 sample/min. PMID:14698236

  9. Estimation of brassylic acid by gas chromatography-mass spectrometry

    SciTech Connect

    Mohammed J. Nasrullah, Erica N. Pfarr, Pooja Thapliyal, Nicholas S. Dusek, Kristofer L. Schiele, Christy Gallagher-Lein, and James A. Bahr

    2010-10-29

    The main focus of this work is to estimate Brassylic Acid (BA) using gas chromatography-mass spectrometry (GC-MS). BA is a product obtained from the oxidative cleavage of Erucic Acid (EA). BA has various applications for making nylons and high performance polymers. BA is a 13 carbon compound with two carboxylic acid functional groups at the terminal end. BA has a long hydrocarbon chain that makes the molecule less sensitive to some of the characterization techniques. Although BA can be characterized by NMR, both the starting material (EA) and products BA and nonanoic acid (NA) have peaks at similar {delta}, ppm values. Hence it becomes difficult for the quick estimation of BA during its synthesis.

  10. Fragmentation energy index for universalization of fragmentation energy in ion trap mass spectrometers for the analysis of chemical weapon convention related chemicals by atmospheric pressure ionization-tandem mass spectrometry analysis.

    PubMed

    Palit, Meehir; Mallard, Gary

    2009-04-01

    The use of mass spectra generated at 70 eV in electron ionization (EI) as a universal standard for EI has helped in the generation of searchable library databases and had a profound influence on the analytical applications of gas chromatography/mass spectrometry (GC/MS), similarly for liquid chromatography tandem mass spectrometry (LC-MS/MS), suggesting a novel method to normalize the collisional energy for the universalization of fragmentation energy for the analysis of Chemical Weapon Convention (CWC)-related chemicals by atmospheric pressure ionization-tandem mass spectrometry (API-MS(n)) using three-dimensional (3D) ion trap instruments. For normalizing fragmentation energy a "fragmentation energy index" (FEI) is proposed which is an arbitrary scale based on the fact of specific MS/MS fragmentation obtained at different collisional energies for the reference chemicals which are not CWC scheduled compounds. FEI 6 for the generation of an MS(n) library-searchable mass spectral database is recommended. PMID:19331429

  11. Development and validation of a new analytical method for the determination of 1,4-dichlorobenzene in honey by gas chromatography-isotope dilution mass spectrometry after steam-distillation.

    PubMed

    Botitsi, E V; Kormali, P N; Kontou, S N; Economou, A; Tsipi, D F

    2006-10-01

    A simple, fast, sensitive and robust analytical method using gas chromatography (GC)-isotope dilution mass spectrometry (MS) was developed and validated for the identification and quantification of 1,4-dichlorobenzene (p-DCB) residues in honey samples. The proposed methodology is based on steam-distillation using a Clevenger-type apparatus followed by gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring (SIM) mode employing the isotopically labeled analogue d4-1,4-dichlorobenzene (d4-p-DCB) as internal standard (IS). Validation of the method was performed in two different GC-MS systems, using quadrupole MS (QMS) and ion-trap MS (ITMS) detectors, with no statistically significant differences between two. Recoveries were better than 91% with percent relative standard deviations lower than 12%. The instrumental limits of detection were 1 microg kg(-1) in the GC-ITMS system and 0.6 microg kg(-1) in the GC-QMS system. The expanded uncertainty was estimated as 17% at the currently accepted "action level" of 10 microg kg(-1). The method was applied to the analysis of 310 honey samples in an extensive national monitoring study. A quality control (QC) system applied during the assays has demonstrated a good performance and long-term stability over a period of more than 8 months of continuous operation. PMID:17723727

  12. Fluorescence imaging for visualization of the ion cloud in a quadrupole ion trap mass spectrometer.

    PubMed

    Talbot, Francis O; Sciuto, Stephen V; Jockusch, Rebecca A

    2013-12-01

    Laser-induced fluorescence is used to visualize populations of gaseous ions stored in a quadrupole ion trap (QIT) mass spectrometer. Presented images include the first fluorescence image of molecular ions collected under conditions typically used in mass spectrometry experiments. Under these "normal" mass spectrometry conditions, the radial (r) and axial (z) full-width at half maxima (FWHM) of the detected ion cloud are 615 and 214 μm, respectively, corresponding to ~6% of r0 and ~3% of z0 for the QIT used. The effects on the shape and size of the ion cloud caused by varying the pressure of helium bath gas, the number of trapped ions, and the Mathieu parameter q z are visualized and discussed. When a "tickle voltage" is applied to the exit end-cap electrode, as is done in collisionally activated dissociation, a significant elongation in the axial, but not the radial, dimension of the ion cloud is apparent. Finally, using spectroscopically distinguishable fluorophores of two different m/z values, images are presented that illustrate stratification of the ion cloud; ions of lower m/z (higher qz) are located in the center of the trapping region, effectively excluding higher m/z (lower qz) ions, which form a surrounding layer. Fluorescence images such as those presented here provide a useful reference for better understanding the collective behavior of ions in radio frequency (rf) trapping devices and how phenomena such as collisions and space-charge affect ion distribution. PMID:24092629

  13. Fluorescence Imaging for Visualization of the Ion Cloud in a Quadrupole Ion Trap Mass Spectrometer

    NASA Astrophysics Data System (ADS)

    Talbot, Francis O.; Sciuto, Stephen V.; Jockusch, Rebecca A.

    2013-12-01

    Laser-induced fluorescence is used to visualize populations of gaseous ions stored in a quadrupole ion trap (QIT) mass spectrometer. Presented images include the first fluorescence image of molecular ions collected under conditions typically used in mass spectrometry experiments. Under these "normal" mass spectrometry conditions, the radial ( r) and axial ( z) full-width at half maxima (FWHM) of the detected ion cloud are 615 and 214 μm, respectively, corresponding to ~6 % of r 0 and ~3 % of z 0 for the QIT used. The effects on the shape and size of the ion cloud caused by varying the pressure of helium bath gas, the number of trapped ions, and the Mathieu parameter q z are visualized and discussed. When a "tickle voltage" is applied to the exit end-cap electrode, as is done in collisionally activated dissociation, a significant elongation in the axial, but not the radial, dimension of the ion cloud is apparent. Finally, using spectroscopically distinguishable fluorophores of two different m/ z values, images are presented that illustrate stratification of the ion cloud; ions of lower m/ z (higher q z ) are located in the center of the trapping region, effectively excluding higher m/ z (lower q z ) ions, which form a surrounding layer. Fluorescence images such as those presented here provide a useful reference for better understanding the collective behavior of ions in radio frequency (rf) trapping devices and how phenomena such as collisions and space-charge affect ion distribution.

  14. Analysis of odour compounds from scented consumer products using gas chromatography-mass spectrometry and gas chromatography-olfactometry.

    PubMed

    Bartsch, Jennifer; Uhde, Erik; Salthammer, Tunga

    2016-01-21

    Scented consumer products are being bought in increasing amounts and gaining more popularity. There is, however, relatively little information available about their ingredients, emissions and allergenic potential. Frequently, a mixture of different fragrance substances and not solely an individual substance contributes to the overall desired smell. The aim of this study was to investigate the odorous volatile organic compounds (OVOCs) in consumer products containing fragrances. Over 44 products were selected: various scented candles, printing products with different scent types and other products types particularly meant to be used indoors. Measurements were carried out in a desiccator. Air samples were collected on thermal desorption tubes to determine the released fragrance substances by means of gas chromatography-mass spectrometry (GC-MS). Moreover, gas chromatography-olfactometry (GC-O) was used to obtain sensory data and to ensure no important odorant was overlooked. Using both methods it was possible to distinguish between odour active and inactive compounds and subsequently to identify almost 300 different odorants across all scented products. Besides the advantage of differentiation, as the human nose is a very sensitive detector, GC-O was found to be a useful tool for detecting traces and chosen target compounds. One focus in this study lay on the 26 EU-regulated fragrance allergens to prove their relevance in scented consumer goods. In total, 18 of them were identified, with at least one substance being present in almost every product. Benzyl alcohol, cinnamaldehyde, citronellol, eugenol, linalool and limonene were the prevalently detected allergens. Particularly linalool and limonene were observed in over 50% of the products. In addition, eugenol appeared to be one of the most frequently detected compounds in trace-level concentrations in the candle emissions. PMID:26724768

  15. Chemical Discrimination in Turbulent Gas Mixtures with MOX Sensors Validated by Gas Chromatography-Mass Spectrometry

    PubMed Central

    Fonollosa, Jordi; Rodríguez-Luján, Irene; Trincavelli, Marco; Vergara, Alexander; Huerta, Ramón

    2014-01-01

    Chemical detection systems based on chemo-resistive sensors usually include a gas chamber to control the sample air flow and to minimize turbulence. However, such a kind of experimental setup does not reproduce the gas concentration fluctuations observed in natural environments and destroys the spatio-temporal information contained in gas plumes. Aiming at reproducing more realistic environments, we utilize a wind tunnel with two independent gas sources that get naturally mixed along a turbulent flow. For the first time, chemo-resistive gas sensors are exposed to dynamic gas mixtures generated with several concentration levels at the sources. Moreover, the ground truth of gas concentrations at the sensor location was estimated by means of gas chromatography-mass spectrometry. We used a support vector machine as a tool to show that chemo-resistive transduction can be utilized to reliably identify chemical components in dynamic turbulent mixtures, as long as sufficient gas concentration coverage is used. We show that in open sampling systems, training the classifiers only on high concentrations of gases produces less effective classification and that it is important to calibrate the classification method with data at low gas concentrations to achieve optimal performance. PMID:25325339

  16. Chemical discrimination in turbulent gas mixtures with MOX sensors validated by gas chromatography-mass spectrometry.

    PubMed

    Fonollosa, Jordi; Rodríguez-Luján, Irene; Trincavelli, Marco; Vergara, Alexander; Huerta, Ramón

    2014-01-01

    Chemical detection systems based on chemo-resistive sensors usually include a gas chamber to control the sample air flow and to minimize turbulence. However, such a kind of experimental setup does not reproduce the gas concentration fluctuations observed in natural environments and destroys the spatio-temporal information contained in gas plumes. Aiming at reproducing more realistic environments, we utilize a wind tunnel with two independent gas sources that get naturally mixed along a turbulent flow. For the first time, chemo-resistive gas sensors are exposed to dynamic gas mixtures generated with several concentration levels at the sources. Moreover, the ground truth of gas concentrations at the sensor location was estimated by means of gas chromatography-mass spectrometry. We used a support vector machine as a tool to show that chemo-resistive transduction can be utilized to reliably identify chemical components in dynamic turbulent mixtures, as long as sufficient gas concentration coverage is used. We show that in open sampling systems, training the classifiers only on high concentrations of gases produces less effective classification and that it is important to calibrate the classification method with data at low gas concentrations to achieve optimal performance. PMID:25325339

  17. Gas phase chromatography of halides of elements 104 and 105

    SciTech Connect

    Tuerler, A.; Gregorich, K.E.; Czerwinski, K.R.; Hannink, N.J.; Henderson, R.A.; Hoffman, D.C.; Kacher, C.D.; Kadkhodayan, B.; Kreek, S.A.; Lee, D.M.; Leyba, J.D.; Nurmia, M.J. ); Gaeggeler, H.W.; Jost, D.T.; Kovacs, J.; Scherer, U.W.; Vermeulen, D.; Weber, A. , Villigen ); Barth, H.; Gober, M.K.; Kratz, J.V. (Philipps-Univ., Marburg

    1991-04-01

    On-line isothermal gas phase chromatography was used to study halides of {sup 261}104 (T{sub {1/2}} = 65 s) and {sup 262,263}105 (T{sub {1/2}} = 34 s and 27 s) produced an atom-at-a time via the reactions {sup 248}Cm({sup 18}O, 5n) and {sup 249}Bk({sup 18}O, 5n, 4n), respectively. Using HBr and HCl gas as halogenating agents, we were able to produce volatile bromides and chlorides of the above mentioned elements and study their behavior compared to their lighter homologs in Groups 4 or 5 of the periodic table. Element 104 formed more volatile bromides than its homolog Hf. In contrast, element 105 bromides were found to be less volatile than the bromides of the group 5 elements Nb and Ta. Both 104 and Hf chlorides were observed to be more volatile than their respective bromides. 31 refs., 8 figs.

  18. Rapid screening of transferrin-binders in the flowers of Bauhinia blakeana Dunn by on-line high-performance liquid chromatography-diode-array detector-electrospray ionization-ion-trap-time-of-flight-mass spectrometry-transferrin-fluorescence detection system.

    PubMed

    Liu, Meixian; Dong, Jing; Lin, Zongtao; Niu, Yanyan; Zhang, Xiaotian; Jiang, Haixiu; Guo, Ning; Li, Wei; Wang, Hong; Chen, Shizhong

    2016-06-10

    Transferrin (Transferrin, TRF, TF) has drawn increasing attention in cancer therapy due to its potential applications in drug delivery. TF receptor, highly expressed in tumor cells, recognizes and transports Fe(3+)-TF into cells to release iron into cytoplasm. Thus, discovering TF-binding compounds has become an active research area and is of great importance for target therapy. In this study, an on-line analysis method was established for screening TF-binding compounds from the flowers of Bauhinia blakeana Dunn using a high-performance liquid chromatography-diode-array detector-multi-stage mass spectrometry-transferrin-fluorescence detector (HPLC-DAD-MS(n)-TF-FLD) method. As a result, 33 of 80 identified or tentatively characterized compounds in the sample were TF-binding active. Twenty-five flavonol glycosides and eight phenolic acids were identified as TF-binders. Twelve of these active compounds together with six standard compounds were used to study the dose-response effects and structure-activity relationships of flavonoids and phenolic acids. The method was validated by vitexin with a good linearity in the range of concentrations used in the study. The limit of detection for vitexin was 0.1596 nmol. Our study indicated that the established method is simple, rapid and sensitive for screening TF-binding active compounds in the extract of Bauhinia blakeana Dunn, and therefore is important for discovering potential anti-cancer ingredients from complex samples for TF related drug delivery. PMID:27178150

  19. Thermal Independent Modulator for Comprehensive Two-Dimensional Gas Chromatography.

    PubMed

    Luong, Jim; Guan, Xiaosheng; Xu, Shifen; Gras, Ronda; Shellie, Robert A

    2016-09-01

    We introduce a modulation strategy for comprehensive two-dimensional gas chromatography (GC×GC) with complete thermal independence between the cooling and heating stages and without the need for GC oven heat for remobilization. Based on this approach, a compact thermal independent modulator (TiM) with thermoelectric cooling and micathermic heating has been successfully innovated for use in GC×GC. The device operates externally to a gas chromatograph, does not require liquid cryogen, and has minimal consumables requirements. The augmentation of an additional gas flow stream results in a number of critical chromatographic parameter improvements such as the decoupling of flows of first- and second-dimension columns to attain both efficiency and speed optimized flow in each dimension, the potential for independent retention time locking or scaling in either dimension, the improvement of modulator reinjection efficiency, as well as facilitating back-flushing for the first dimension to enhance system cleanliness and throughput. TiM was found to be useful for chromatographic applications over a volatility range equivalent to nC6 to nC24 under conditions used. Repeatability of retention time for model compounds such as benzene, toluene, ethyl benzene, and xylenes were found to be quite satisfactory with relative standard deviations of less than 0.009% in (1)D and less than 0.008% in (2)D (n = 10). Typical peak widths of 120 ms or less with a relative standard deviation of less than 4.7% were achieved for the aromatic model compounds. In this article, the performance of the modulator is demonstrated and a series of challenging chromatographic applications are presented to illustrate usefulness of the apparatus. PMID:27537206

  20. Characteristics of Ion Activation and Collision Induced Dissociation Using Digital Ion Trap Technology.

    PubMed

    Xu, Fuxing; Dang, Qiankun; Dai, Xinhua; Fang, Xiang; Wang, Yuanyuan; Ding, Li; Ding, Chuan-Fan

    2016-08-01

    Collision induced dissociation (CID) is one of the most established techniques for tandem mass spectrometry analysis. The CID of mass selected ion could be realized by ion resonance excitation with a digital rectangular waveform. The method is simple, and highly efficient CID result could be obtained by optimizing the experimental parameters, such as digital waveform voltage, frequency, and q value. In this work, the relationship between ion trapping waveform voltage and frequency at preselected q value, the relationship between waveform frequency and the q value at certain ion trapping voltage for optimum CID efficiency were investigated. Experiment results showed that the max CID efficiency of precursor reserpine ions can be obtained at different trapping waveform voltage and frequency when q and β are different. Based on systematic experimental analysis, the optimum experimental conditions for high CID efficiency can be calculated at any selected β or q. By using digital ion trap technology, the CID process and efficient fragmentation of parent ions can be realized by simply changing the trapping waveform amplitude, frequency, and the β values in the digital ion trap mass spectrometry. The technology and method are simple. It has potential use in ion trap mass spectrometry. Graphical Abstract ᅟ. PMID:27150507

  1. Multiple Mass Analysis Using an Ion Trap Array (ITA) Mass Analyzer

    NASA Astrophysics Data System (ADS)

    Xiao, Yu; Chu, Yanqiu; Ling, Xing; Ding, Zhengzhi; Xu, Chongsheng; Ding, Li; Ding, Chuan-Fan

    2013-09-01

    A novel ion trap array (ITA) mass analyzer with six ion trapping and analyzing channels was investigated. It is capable of analyzing multiple samples simultaneously. The ITA was built with several planar electrodes made of stainless steel and 12 identical parallel zirconia ceramic substrates plated with conductive metal layers. Each two of the opposing ceramic electrode plates formed a boundary of an ion trap channel and six identical ion trapping and analyzing channels were placed in parallel without physical electrode between any two adjacent channels. The electric field distribution inside each channel was studied with simulation. The new design took the advantage of high precision machining attributable to the rigidity of ceramic, and the convenience of surface patterning technique. The ITA system was tested by using a two-channel electrospray ionization source, a multichannel simultaneous quadruple ion guide, and two detectors. The simultaneous analysis of two different samples with two adjacent ITA channels was achieved and independent mass spectra were obtained. For each channel, the mass resolution was tested. Additional ion trap functions such as mass-selected ion isolation and collision-induced dissociation (CID) were also tested. The results show that one ITA is well suited for multiple simultaneous mass analyses.

  2. Characteristics of Ion Activation and Collision Induced Dissociation Using Digital Ion Trap Technology

    NASA Astrophysics Data System (ADS)

    Xu, Fuxing; Dang, Qiankun; Dai, Xinhua; Fang, Xiang; Wang, Yuanyuan; Ding, Li; Ding, Chuan-Fan

    2016-08-01

    Collision induced dissociation (CID) is one of the most established techniques for tandem mass spectrometry analysis. The CID of mass selected ion could be realized by ion resonance excitation with a digital rectangular waveform. The method is simple, and highly efficient CID result could be obtained by optimizing the experimental parameters, such as digital waveform voltage, frequency, and q value. In this work, the relationship between ion trapping waveform voltage and frequency at preselected q value, the relationship between waveform frequency and the q value at certain ion trapping voltage for optimum CID efficiency were investigated. Experiment results showed that the max CID efficiency of precursor reserpine ions can be obtained at different trapping waveform voltage and frequency when q and β are different. Based on systematic experimental analysis, the optimum experimental conditions for high CID efficiency can be calculated at any selected β or q. By using digital ion trap technology, the CID process and efficient fragmentation of parent ions can be realized by simply changing the trapping waveform amplitude, frequency, and the β values in the digital ion trap mass spectrometry. The technology and method are simple. It has potential use in ion trap mass spectrometry.

  3. Characteristics of Ion Activation and Collision Induced Dissociation Using Digital Ion Trap Technology

    NASA Astrophysics Data System (ADS)

    Xu, Fuxing; Dang, Qiankun; Dai, Xinhua; Fang, Xiang; Wang, Yuanyuan; Ding, Li; Ding, Chuan-Fan

    2016-05-01

    Collision induced dissociation (CID) is one of the most established techniques for tandem mass spectrometry analysis. The CID of mass selected ion could be realized by ion resonance excitation with a digital rectangular waveform. The method is simple, and highly efficient CID result could be obtained by optimizing the experimental parameters, such as digital waveform voltage, frequency, and q value. In this work, the relationship between ion trapping waveform voltage and frequency at preselected q value, the relationship between waveform frequency and the q value at certain ion trapping voltage for optimum CID efficiency were investigated. Experiment results showed that the max CID efficiency of precursor reserpine ions can be obtained at different trapping waveform voltage and frequency when q and β are different. Based on systematic experimental analysis, the optimum experimental conditions for high CID efficiency can be calculated at any selected β or q. By using digital ion trap technology, the CID process and efficient fragmentation of parent ions can be realized by simply changing the trapping waveform amplitude, frequency, and the β values in the digital ion trap mass spectrometry. The technology and method are simple. It has potential use in ion trap mass spectrometry.

  4. Multiple mass analysis using an ion trap array (ITA) mass analyzer.

    PubMed

    Yu, Xiao; Chu, Yanqiu; Ling, Xing; Ding, Zhengzhi; Xu, Chongsheng; Ding, Li; Ding, Chuan-Fan

    2013-09-01

    A novel ion trap array (ITA) mass analyzer with six ion trapping and analyzing channels was investigated. It is capable of analyzing multiple samples simultaneously. The ITA was built with several planar electrodes made of stainless steel and 12 identical parallel zirconia ceramic substrates plated with conductive metal layers. Each two of the opposing ceramic electrode plates formed a boundary of an ion trap channel and six identical ion trapping and analyzing channels were placed in parallel without physical electrode between any two adjacent channels. The electric field distribution inside each channel was studied with simulation. The new design took the advantage of high precision machining attributable to the rigidity of ceramic, and the convenience of surface patterning technique. The ITA system was tested by using a two-channel electrospray ionization source, a multichannel simultaneous quadruple ion guide, and two detectors. The simultaneous analysis of two different samples with two adjacent ITA channels was achieved and independent mass spectra were obtained. For each channel, the mass resolution was tested. Additional ion trap functions such as mass-selected ion isolation and collision-induced dissociation (CID) were also tested. The results show that one ITA is well suited for multiple simultaneous mass analyses. PMID:23797864

  5. Preparation of fatty acid methyl esters for gas-liquid chromatography[S

    PubMed Central

    Ichihara, Ken'ichi; Fukubayashi, Yumeto

    2010-01-01

    A convenient method using commercial aqueous concentrated HCl (conc. HCl; 35%, w/w) as an acid catalyst was developed for preparation of fatty acid methyl esters (FAMEs) from sterol esters, triacylglycerols, phospholipids, and FFAs for gas-liquid chromatography (GC). An 8% (w/v) solution of HCl in methanol/water (85:15, v/v) was prepared by diluting 9.7 ml of conc. HCl with 41.5 ml of methanol. Toluene (0.2 ml), methanol (1.5 ml), and the 8% HCl solution (0.3 ml) were added sequentially to the lipid sample. The final HCl concentration was 1.2% (w/v). This solution (2 ml) was incubated at 45°C overnight or heated at 100°C for 1–1.5 h. The amount of FFA formed in the presence of water derived from conc. HCl was estimated to be <1.4%. The yields of FAMEs were >96% for the above lipid classes and were the same as or better than those obtained by saponification/methylation or by acid-catalyzed methanolysis/methylation using commercial anhydrous HCl/methanol. The method developed here could be successfully applied to fatty acid analysis of various lipid samples, including fish oils, vegetable oils, and blood lipids by GC. PMID:19759389

  6. A Novel Dual-Pressure Linear Ion Trap Mass Spectrometer Improves the Analysis of Complex Protein Mixtures

    PubMed Central

    Pekar, Tonya; Blethrow, Justin D.; Schwartz, Jae C.; Merrihew, Gennifer E.; MacCoss, Michael J.; Swaney, Danielle L.; Russell, Jason D.; Coon, Joshua J.; Zabrouskov, Vlad

    2009-01-01

    The considerable progress in high throughput proteomics analysis via liquid chromatography-electrospray ionization-tandem mass spectrometry over the last decade has been fueled to a large degree by continuous improvements in instrumentation. High throughput identification experiments are based on peptide sequencing and are largely accomplished through the use of tandem mass spectrometry, with ion trap and trap-based instruments having become broadly adopted analytical platforms. To satisfy increasingly demanding requirements for depth of characterization and throughput, we present a newly developed dual-pressure linear ion trap mass spectrometer (LTQ Velos) that features increased sensitivity, afforded by a new source design, and demonstrates practical cycle times two times shorter than that of an LTQ XL, while improving or maintaining spectral quality for MS/MS fragmentation spectra. These improvements resulted in a substantial increase in the detection and identification of both proteins and unique peptides from the complex proteome of Caenorhabditis elegans, as compared to existing platforms. The greatly increased ion flux into the mass spectrometer in combination with improved isolation of low-abundance precursor ions resulted in increased detection of low-abundance peptides. These improvements cumulatively resulted in a substantially greater penetration into the baker’s yeast (Saccharomyces cerevisiae) proteome compared to LTQ XL. Alternatively, faster cycle times on the new instrument allowed for higher throughput for a given depth of proteome analysis, with more peptides and proteins identified in 60 min using an LTQ Velos than in 180 min using an LTQ XL. When mass analysis was carried out with resolution in excess of 25,000 FWHM, it became possible to isotopically resolve a small intact protein and its fragments, opening possibilities for top down experiments. PMID:19689114

  7. The ReA electron-beam ion trap charge breeder for reacceleration of rare isotopes

    SciTech Connect

    Lapierre, A.; Schwarz, S.; Kittimanapun, K.; Fogleman, J.; Krause, S.; Nash, S.; Rencsok, R.; Tobos, L.; Perdikakis, G.; Portillo, M.; Rodriguez, J. A.; Wittmer, W.; Wu, X.; Bollen, G.; Leitner, D.; Syphers, M.; Collaboration: ReA Team

    2013-04-19

    ReA is a post-accelerator at the National Superconducting Cyclotron Laboratory at Michigan State University. ReA is designed to reaccelerate rare isotopes to energies of a few MeV/u following production by projectile fragmentation and thermalization in a gas cell. The facility consists of four main components: an electron-beam ion trap (EBIT) charge breeder, an achromatic charge-over-mass (Q/A) separator, a radio-frequency quadrupole accelerator, and a superconducting radio-frequency linear accelerator. The EBIT charge breeder was specifically designed to efficiently capture continuous beams of singly charged ions injected at low energy (<60 keV), charge breed in less than 50 ms, and extract highly charged ions to the Q/A separator for charge-state selection and reacceleration through the accelerator structures. The use of highly charged ions to reach high beam energies is a key aspect that makes ReA a compact and cost-efficient post-accelerator. The EBIT is characterized by a high-current electron gun, a long multi-electrode trap structure and a dual magnet to provide both the high electron-beam current density necessary for fast charge breeding of short-lived isotopes as well as the high capture probability of injected beams. This paper presents an overview and the status of the ReA EBIT, which has extracted for reacceleration tests stable {sup 20}Ne{sup 8+} ion beams produced from injected gas and more recently {sup 39}K{sup 16+} beams by injecting stable {sup 39,41}K{sup +} ions from an external ion source.

  8. The ReA electron-beam ion trap charge breeder for reacceleration of rare isotopes

    NASA Astrophysics Data System (ADS)

    Lapierre, A.; Schwarz, S.; Kittimanapun, K.; Fogleman, J.; Krause, S.; Nash, S.; Rencsok, R.; Tobos, L.; Perdikakis, G.; Portillo, M.; Rodriguez, J. A.; Wittmer, W.; Wu, X.; Bollen, G.; Leitner, D.; Syphers, M.; ReA Team

    2013-04-01

    ReA is a post-accelerator at the National Superconducting Cyclotron Laboratory at Michigan State University. ReA is designed to reaccelerate rare isotopes to energies of a few MeV/u following production by projectile fragmentation and thermalization in a gas cell. The facility consists of four main components: an electron-beam ion trap (EBIT) charge breeder, an achromatic charge-over-mass (Q/A) separator, a radio-frequency quadrupole accelerator, and a superconducting radio-frequency linear accelerator. The EBIT charge breeder was specifically designed to efficiently capture continuous beams of singly charged ions injected at low energy (<60 keV), charge breed in less than 50 ms, and extract highly charged ions to the Q/A separator for charge-state selection and reacceleration through the accelerator structures. The use of highly charged ions to reach high beam energies is a key aspect that makes ReA a compact and cost-efficient post-accelerator. The EBIT is characterized by a high-current electron gun, a long multi-electrode trap structure and a dual magnet to provide both the high electron-beam current density necessary for fast charge breeding of short-lived isotopes as well as the high capture probability of injected beams. This paper presents an overview and the status of the ReA EBIT, which has extracted for reacceleration tests stable 20Ne8+ ion beams produced from injected gas and more recently 39K16+ beams by injecting stable 39,41K+ ions from an external ion source.

  9. T-junction ion trap array for two-dimensional ion shuttling, storage, and manipulation

    SciTech Connect

    Hensinger, W.K.; Olmschenk, S.; Stick, D.; Hucul, D.; Yeo, M.; Acton, M.; Deslauriers, L.; Monroe, C.; Rabchuk, J.

    2006-01-16

    We demonstrate a two-dimensional 11-zone ion trap array, where individual laser-cooled atomic ions are stored, separated, shuttled, and swapped. The trap geometry consists of two linear rf-ion trap sections that are joined at a 90 deg. angle to form a T-shaped structure. We shuttle a single ion around the corners of the T-junction and swap the positions of two crystallized ions using voltage sequences designed to accommodate the nontrivial electrical potential near the junction. Full two-dimensional control of multiple ions demonstrated in this system may be crucial for the realization of scalable ion trap quantum computation and the implementation of quantum networks.

  10. A quadrupole ion trap with cylindrical geometry operated in the mass-selective instability mode.

    PubMed

    Wells, J M; Badman, E R; Cooks, R G

    1998-02-01

    A cylindrical geometry ion trap is used to record mass spectra in the mass-selective instability mode. The geometry of the cylindrical ion trap has been optimized to maximize the quadrupole field component relative to the higher-order field content through field calculations using the Poisson/Superfish code and through experimental variation of the electrode structure. The results correspond well with predictions of the calculations. The trap has been used to record mass spectra with better than unit mass resolution, high sensitivity, and a mass/charge range of ∼600 Th. Multistage (MS(3)) experiments have been performed, and the Mathieu stability region has been experimentally mapped. The performance of this device compares satisfactorily with that of the hyperbolic ion trap. PMID:21644742

  11. Advances in ion trap mass spectrometry: Photodissociation as a tool for structural elucidation

    SciTech Connect

    Stephenson, J.L. Jr.; Booth, M.M.; Eyler, J.R.; Yost, R.A.

    1995-12-01

    Photo-induced dissociation (PID) is the next most frequently used method (after collisional activation) for activation of Polyatomic ions in tandem mass spectrometry. The range of internal energies present after the photon absorption process are much narrower than those obtained with collisional energy transfer. Therefore, the usefulness of PID for the study of ion structures is greatly enhanced. The long storage times and instrumental configuration of the ion trap mass spectrometer are ideally suited for photodissociation experiments. This presentation will focus on both the fundamental and analytical applications of CO{sub 2} lasers in conjunction with ion trap mass spectrometry. The first portion of this talk will examine the fundamental issues of wavelength dependence, chemical kinetics, photoabsorption cross section, and collisional effects on photodissociation efficiency. The second half of this presentation will look at novel instrumentation for electrospray/ion trap mass spectrometry, with the concurrent development of photodissociation as a tool for structural elucidation of organic compounds and antibiotics.

  12. Ion collision crosssection measurements in quadrupole ion traps using a time-frequency analysis method.

    PubMed

    He, Muyi; Guo, Dan; Chen, Yu; Xiong, Xingchuang; Fang, Xiang; Xu, Wei

    2014-12-01

    In this study, a method for measuring ion collision crosssections (CCSs) was proposed through time-frequency analysis of ion trajectories in quadrupole ion traps. A linear ion trap with added high-order electric fields was designed and simulated. With the presence of high-order electric fields and ion-neutral collisions, ion secular motion frequency within the quadrupole ion trap will be a function of ion motion amplitude, thus a function of time and ion CCS. A direct relationship was then established between ion CCS and ion motion frequency with respect to time, which could be obtained through time-frequency analysis of ion trajectories (or ion motion induced image currents). To confirm the proposed theory, realistic ion trajectory simulations were performed, where the CCSs of bradykinin, angiotensin I and II, and ubiquitin ions were calculated from simulated ion trajectories. As an example, differentiation of isomeric ubiquitin ions was also demonstrated in the simulations. PMID:25319271

  13. [Determination of dimethylbenzoic acid isomers in urine by gas chromatography].

    PubMed

    Kostrzewski, P; Wiaderna-Brycht, A; Czerski, B

    1994-01-01

    Trimethylobenzene (TMB) is a main ingredient of many organic solvents used in industry. In Farbasol (Polish trade name of the solvent) TMB occurs as a mixture of three isomers: pseudocumene (1, 2, 4-TMB) 30%; mesitylene (1, 3, 5-TMB) 15%; hemimellitene (1,2,3-TMB) 5%. As it is known in human organism, TMB is metabolized mainly to dimethylbenzoic (DMBA) and dimethylhippuric (DMHA) acids, and some authors suggest, that the acids excreted in urine can be biological indicators of exposure to TMB. This study was aimed at developing the method of determination of DMBA isomers in urine. Biological material was hydrolyzed with sodium hydroxide and next extracted with diethyl ether. DMBA concentration in urine was determined by gas chromatography using a variant of quantitative analysis with internal standard (5-methyl-2-isopropylphenol, thymol). Analytical parameters of the developed method of determination of DMBA isomers in urine such as linearity, precision, reproducibility, stability (192 days, when urine samples stored at-18 degrees C), detectability limit (400 micrograms/dm3) have been fully compatible with the requirements of biological monitoring. In order to confirm the presence of DMBA isomers in urine, four volunteers were exposed (8 hours) to Farbasol in toxicological chamber. The TMB concentration in the air, determined by means of gas chromatograph (HP 5890), amounted to 100 mg/m3 (MAC value in Poland). In urine samples collected 2,3-; 2,4-; 2,5-; 2,6-; 3,4-; 3,5-dimethylbenzoic acids were identified by means of GC/MSD.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:8170375

  14. Determination of thermal stability of oils by pyrolytic gas chromatography

    SciTech Connect

    Kudryavtseva, N.A.; Mikhailov, I.A.; Nikonorov, E.M.; Rakova, L.A.

    1984-03-01

    This article demonstrates how pyrolytic gas chromatography (PGC) offers a means for unambiguous differentiation of the decomposition products from the accompanying products of oil vaporization. The proposed method based on PGC uses a furnace-type pyrolyzer connected to an LKhM-7A chromatograph. The common peak of propane with propylene was selected as a characteristic peak to indicate the oil decomposition temperature. Propane and propylene, along with lighter hydrocarbons, are always present in the decomposition products. A volume graph method is used to determine the temperature of vaporization or decomposition of the substance, based on plotting a curve for the relationship between the heating temperature and the relative volume (or pressure) of the test sample. The decomposition temperatures determined by the PGC method agree with the values report by foreign manufacturers (deviation no greater than 2/sup 0/C). The accuracy of calculation of the thermal stability of the hydrocarbon oils by the PGC method was 5-10/sup 0/C as a result of deficiencies in the heating device in the pyrolytic unit. Includes a table.

  15. Polyimide polymer glass-free capillary columns for gas chromatography.

    PubMed

    Webster, Jackie G; Marine, Susan S; Danielson, Neil D

    2011-01-01

    Polymeric polyimide capillary tubing, both uncoated and coated with stationary phases of two polarities, is explored for use as capillary columns for gas chromatography (GC). These glass-free polyimide columns are flexible and their small winding diameter of less than a cm around a solid support makes them compatible for potential use in portable GC instruments. Polyimide columns with dimensions of 0.32 mm i.d. × 3 m are cleaned, annealed at 300°C, and coated using the static method with phenylmethylsilicone (PMS). Separations of volatile organics are investigated isothermally on duplicate sets of polyimide columns by GC with a flame ionization detector using split injection. Unlike the uncoated ones, the coated polyimide columns successfully separate Grob test mix classes of alkanes, amines, and fatty acid methyl esters. The relative standard deviations for retention time and peak area are 0.5 and 2.5 , respectively. With the 3 m PMS-coated column connected to a retention gap to permit operation at its optimum flow rate of 30 cm/s, a plate count of 3200 or plate height of 1 mm is possible. Lack of retention and tailing peaks are evident for the polyimide polymer capillary columns as compared to that of a 3 m commercial cross-linked PMS fused silica capillary. However, headspace analyses of an aromatic hydrocarbon mix and a Clearcoat automotive paint sample are viable applications on the PMS polyimide polymer column. PMID:21682994

  16. Quantitative analysis of terbutaline by gas chromatography-mass spectrometry.

    PubMed

    Leferink, J G; Baillie, T A; Lindberg, C

    1984-01-01

    Over the past 6 years, several gas chromatography-mass spectrometry (GC-MS) methods for terbutaline have been developed, each with certain advantages and disadvantages. They all involve monitoring of an ion selected from the mass spectrum of a suitable terbutaline derivative. This technique, often referred to as mass fragmentography or selected ion monitoring, reduces the interference from other drugs and endogenous compounds. Different ionization techniques have been employed to obtain high sensitivity, viz. electron impact and chemical ionization. Typically, the methods can be used to measure terbutaline concentrations down to 0.1-0.3 ng/mL in plasma or serum. Isolation of terbutaline from biological materials is complicated by the low partition of the drug from water to organic solvents. Extraction with a large volume of ethyl acetate, ion pair extraction, or isolation on a cation exchange column have been used. These methods are time consuming, and attempts have therefore been made to modify them. Rapid extraction can be achieved on a disposable reversed-phase octadecylsilyl column with unimpaired sensitivity and selectivity. Preliminary results indicate that negative ion chemical ionization of a fluorine-containing derivative can further increase the sensitivity of the terbutaline assays. PMID:6586484

  17. Determination of hair nicotine by gas chromatography-mass spectrometry.

    PubMed

    Man, Che Nin; Ismail, Syazwani; Harn, Gam Lay; Lajis, Razak; Awang, Rahmat

    2009-01-15

    Hair nicotine is a known biomarker for monitoring long-term environmental tobacco smoke (ETS) exposure and smoking status. In general, hair nicotine assay involves alkaline digestion, extraction and instrumental analysis. The gas chromatography-mass spectrometry (GC-MS) assay currently developed has shown to be of high throughput with average approximately 100 hair samples being extracted and analyzed per day. This was achieved through simplified extraction procedure and shortened GC analysis time. The extraction was improved by using small volume (0.4 mL) of organic solvent that does not require further evaporation and salting steps prior to GC-MS analysis. Furthermore, the amount of hair utilized in the extraction was very little (5 mg) while the sensitivity and selectivity of the assay is equal, if not better than other established methods. The linearity of the assay (r(2)>0.995), limit of quantitation (0.04 ng/mg hair), within- and between-assays accuracies and precisions (<11.4%) and mean recovery (92.6%) were within the acceptable range. PMID:19109080

  18. [Enantioseparation of 2-phenylcarboxylic acid esters by capillary gas chromatography].

    PubMed

    Shi, Xueyan; Liu, Feipeng; Bian, Qinghua

    2016-01-01

    Chiral 2-arylcarboxylic acid derivatives are important intermediates for preparing 2-arylcarboxylic acids, which are non-steroidal anti-inflammatory drugs (NSAIDs). In order to separate 2-phenylcarboxylic acid ester enantiomers by capillary gas chromatography (CGC), 2, 6-di-O-pentyl-3-O-butyryl-β-cyclodextrin and 2,6-di-O-benzyl-3-O-heptanoyl-β-cyclodextrin were used as CGC chiral stationary phases, separately, and their enantioseparation abilities to enantiomers of methyl 2-phenylbutanoate, ethyl 2-phenylbutanoate, isopropyl 2-phenylbutanoate, methyl 2-phenylpropionate and cyclopentyl 2-phenylpropionate were examined. It was found that methyl 2-phenylbutanoate, methyl 2-phenylpropionate and cyclopentyl 2-phenylpropionate were successfully separated by using 2,6-di-O-pentyl-3-O-butyryl-β-cyclodextrin and 2,6-di-O-benzyl-3-O-heptanoyl-β-cyclodextrin as CGC chiral stationary phases, respectively. The enantiomer separation abilities of 2, 6-di-O-pentyl-3-O-butyryl-β-cyclodextrin to the three pairs of 2-phenylcarboxylic acid esters tested are superior to those of 2, 6-di-O-benzyl-3-O-heptanoyl-β-cyclodextrin. PMID:27319170

  19. An improved multiple flame photometric detector for gas chromatography.

    PubMed

    Clark, Adrian G; Thurbide, Kevin B

    2015-11-20

    An improved multiple flame photometric detector (mFPD) is introduced, based upon interconnecting fluidic channels within a planar stainless steel (SS) plate. Relative to the previous quartz tube mFPD prototype, the SS mFPD provides a 50% reduction in background emission levels, an orthogonal analytical flame, and easier more sensitive operation. As a result, sulfur response in the SS mFPD spans 4 orders of magnitude, yields a minimum detectable limit near 9×10(-12)gS/s, and has a selectivity approaching 10(4) over carbon. The device also exhibits exceptionally large resistance to hydrocarbon response quenching. Additionally, the SS mFPD uniquely allows analyte emission monitoring in the multiple worker flames for the first time. The findings suggest that this mode can potentially further improve upon the analytical flame response of sulfur (both linear HSO, and quadratic S2) and also phosphorus. Of note, the latter is nearly 20-fold stronger in S/N in the collective worker flames response and provides 6 orders of linearity with a detection limit of about 2.0×10(-13)gP/s. Overall, the results indicate that this new SS design notably improves the analytical performance of the mFPD and can provide a versatile and beneficial monitoring tool for gas chromatography. PMID:25907666

  20. Novel sampling methods for use with thermal desorption ion trap mass spectrometry

    SciTech Connect

    Barshick, S.A.; Buchanan, M.V.

    1994-12-31

    Novel sampling approaches have been investigated to improve the analytical utility of thermal desorption Direct Sampling Ion Trap Mass Spectrometry (DSITMS). Because DSITMS involves the direct introduction of samples into an ion trap mass spectrometer, problems with detection capabilities (sensitivity and selectivity) can often occur when performing trace analysis in complex matrices. Various sampling approaches have been evaluated to improve thermal desorption detection capabilities and to extend the utilities of DSITMS methodologies without significantly increasing analysis times or the cost-effectiveness of DSITMS methods. Three sampling approaches have been investigated including solid phase microextraction (SPME), solid phase extraction columns (SPEC), and purge and trap.

  1. Ion trap mass spectrometric detection of laser desorbed ions from derivatized fused silica fibers

    SciTech Connect

    Garrett, A.W.; Earl, W.L.; Cisper, M.E.; Nogar, N.S.; Hemberger, P.H.

    1994-12-31

    Solid-phase microextraction of analytes from complex matrices using fused silica fibers has many advantages over traditional chemical sample preparation technique. Microextraction requires small sample sizes little sample preparation (providing rapid sample turnaround time), and greatly reduces the amount of chemical waste generated in sample preparation. These advantages make fused silica fibers attractive for direct sampling and detection experiments using laser desorption ion trap mass spectrometry (LITMS). The drawback is the very small area ({approximately}1 mm{sup 2}) exposed to laser irradiation, which limits the amount of material desorbed into the ion trap.

  2. Ion trap mass spectrometry on a comet nucleus: the Ptolemy instrument and the Rosetta space mission.

    PubMed

    Todd, John F J; Barber, Simeon J; Wright, Ian P; Morgan, Geraint H; Morse, Andrew D; Sheridan, Simon; Leese, Mark R; Maynard, Jon; Evans, Suzanne T; Pillinger, Colin T; Drummond, Duncan L; Heys, Samantha C; Huq, S Ejaz; Kent, Barry J; Sawyer, Eric C; Whalley, Martin S; Waltham, Nicholas R

    2007-01-01

    In May 2014, the Rosetta spacecraft is scheduled to rendezvous with the comet Churyumov-Gerasimenko ('67P'). One of the instruments on board the 'Lander' which will descend on to the surface of the comet is a miniaturised GC/MS system that incorporates an ion trap mass spectrometer, specially developed for isotope ratio analysis. This article describes the development and optimisation of the ion trap for this unique application, and presents a summary of the range of pre-programmed experiments that will contribute to the characterisation of the solid and volatile cometary materials. PMID:17154436

  3. Isoconversion effective activation energies derived from repetitive injection fast gas chromatography/mass spectrometry

    NASA Astrophysics Data System (ADS)

    White, Robert L.

    2009-10-01

    Evolved gas analysis by using fast temperature programmed gas chromatography/mass spectrometry is described. A small volume gas chromatograph oven is used to permit rapid heating and cooling of a capillary gas chromatography column, resulting in short analysis cycle times. This capability permits automated sampling and analysis of a purge gas effluent stream generated during thermal analysis of a solid sample. Species-specific mass spectral information extracted from successively acquired chromatograms can be used to generate concentration profiles for volatile products produced during sample heating. These species-specific profiles can be used for calculation of isoconversion effective activation energies that are useful for characterizing the thermal reaction processes.

  4. Prospects for Ultra-Stable Timekeeping with Sealed Vacuum Operation in Multi-Pole Linear Ion Trap Standards

    NASA Technical Reports Server (NTRS)

    Burt, Eric A.; Tjoelker, R. L.

    2007-01-01

    A recent long-term comparison between the compensated multi-pole Linear Ion Trap Standard (LITS) and the laser-cooled primary standards via GPS carrier phase time transfer showed a deviation of less than 2.7x10(exp -17)/day. A subsequent evaluation of potential drift contributors in the LITS showed that the leading candidates are fluctuations in background gases and the neon buffer gas. The current vacuum system employs a "flow-through" turbomolecular pump and a diaphragm fore pump. Here we consider the viability of a "sealed" vacuum system pumped by a non-evaporable getter for long-term ultra-stable clock operation. Initial tests suggests that both further stability improvement and longer mean-time-between-maintenance can be achieved using this approach

  5. DIRECT-DEPOSITION INFRARED SPECTROMETRY WITH GAS AND SUPERCRITICAL FLUID CHROMATOGRAPHY

    EPA Science Inventory

    A direct-deposition Fourier transform infrared (FT-IR) system has been evaluated for applicability to gas chromatography (GC) and supercritical fluid chromatography (SFC) of environmental analytes. A 100-um i.d. fused-silica transfer line was used for GC, and a 50-um transfer lin...

  6. Unexpected dimerization of isoprene in a gas chromatography inlet. A study by gas chromatography/mass spectrometry coupling.

    PubMed

    Estevez, Yannick; Gardrat, Christian; Berthelot, Karine; Grau, Etienne; De Jeso, Bernard; Ouardad, Samira; Peruch, Frédéric

    2014-02-28

    During analysis of pure isoprene by gas chromatography/mass spectrometry (GC-MS) using a programmed temperature vaporization (PTV) inlet, the presence of several isoprene dimers was detected in the total ion chromatograms (TICs). This study intends to determine the part of the instrument where dimerization occurs and the relative importance of the dimer amounts under different experimental conditions. The reference thermal dimerization of isoprene gives four six-membered cyclic dimers and two eight-membered ones. In all samples containing different amounts of freshly distilled isoprene, only peaks corresponding to the former appeared in TICs. For the same temperature, their amounts increase as the concentration of injected isoprene increases. The main products are diprene (from 80 to 100%) of the total dimers and dipentene (from 1 to 14%). The sum of the two other dimers is never higher than 6%. In conclusion, isomeric dimers are produced through a dimerization in the inlet. No dimerization of isoprene occurs in the mass spectrometer source. Then care is needed when analyzing terpenic compounds in the presence of isoprene by GC-MS because structures, retention times and mass spectra of diprene and dipentene are close. PMID:24485537

  7. Chemical Composition of Latent Fingerprints by Gas Chromatography-Mass Spectrometry

    ERIC Educational Resources Information Center

    Hartzell-Baguley, Brittany; Hipp, Rachael E.; Morgan, Neal R.; Morgan, Stephen L.

    2007-01-01

    An experiment in which gas chromatography-mass spectrometry (GC-MS) is used for latent fingerprint extraction and analysis on glass beads or glass slides is conducted. The results determine that the fingerprint residues are gender dependent.

  8. Analysis of chemical signals in red fire ants by gas chromatography and pattern recognition techniques

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The combination of gas chromatography and pattern recognition (GC/PR) analysis is a powerful tool for investigating complicated biological problems. Clustering, mapping, discriminant development, etc. are necessary to analyze realistically large chromatographic data sets and to seek meaningful relat...

  9. Preparation of pure microbiological samples for pyrolysis gas-liquid chromatography studies

    NASA Technical Reports Server (NTRS)

    Oxborrow, G. S.; Fields, N. D.; Puleo, J. R.

    1976-01-01

    Bacterial samples were prepared for pyrolysis gas-liquid chromatography using cells grown on membrane filters. Pyrochromatograms were reproducible when cells harvested from the filters were pyrolyzed without being washed.

  10. ENVIRONMENTAL ANALYSIS BY AB INITIO QUANTUM MECHANICAL COMPUTATION AND GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY.

    EPA Science Inventory

    Computational chemistry, in conjunction with gas chromatography/mass spectrometry/Fourier transform infrared spectrometry (GC/MS/FT-IR), was used to tentatively identify seven tetrachlorobutadiene (TCBD) isomers detected in an environmental sample. Computation of the TCBD infrare...

  11. DETERMINATION OF CHLOROETHENES IN ENVIRONMENTAL BIOLOGICAL SAMPLES USING GAS CHROMATOGRAPHY COUPLED WITH SOLID PHASE MICRO EXTRACTION

    EPA Science Inventory

    An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase mi...

  12. VACUUM DISTILLATION COUPLED WITH GAS CHROMATOGRAPHY/MASS SPECTROMETRY FOR THE ANALYSIS OF ENVIRONMENTAL SAMPLES

    EPA Science Inventory

    A procedure is presented that uses a vacuum distillation/gas chromatography/mass spectrometry system for analysis of problematic matrices of volatile organic compounds. The procedure compensates for matrix effects and provides both analytical results and confidence intervals from...

  13. AN EPA MANUAL FOR ORGANICS ANALYSIS USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    This procedural manual defines the areas of applicability of gas chromatography-mass spectrometry in environmental analysis. The manual includes sample preparation methods specifically adapted to this measurement technique, data processing and interpretation methods, quality cont...

  14. Development of a Linear Ion Trap Mass Spectrometer (LITMS) Investigation for Future Planetary Surface Missions

    NASA Technical Reports Server (NTRS)

    Brinckerhoff, W.; Danell, R.; Van Ameron, F.; Pinnick, V.; Li, X.; Arevalo, R.; Glavin, D.; Getty, S.; Mahaffy, P.; Chu, P.; Zacny, K.; Rogacki, S.; Grubisic, A.; Cornish, T.

    2014-01-01

    Future surface missions to Mars and other planetary bodies will benefit from continued advances in miniature sensor and sample handling technologies that enable high-performance chemical analyses of natural samples. Fine-scale (approx.1 mm and below) analyses of rock surfaces and interiors, such as exposed on a drill core, will permit (1) the detection of habitability markers including complex organics in association with their original depositional environment, and (2) the characterization of successive layers and gradients that can reveal the time-evolution of those environments. In particular, if broad-based and highly-sensitive mass spectrometry techniques could be brought to such scales, the resulting planetary science capability would be truly powerful. The Linear Ion Trap Mass Spectrometer (LITMS) investigation is designed to conduct fine-scale organic and inorganic analyses of short (approx.5-10 cm) rock cores such as could be acquired by a planetary lander or rover arm-based drill. LITMS combines both pyrolysis/gas chromatograph mass spectrometry (GCMS) of sub-sampled core fines, and laser desorption mass spectrometry (LDMS) of the intact core surface, using a common mass analyzer, enhanced from the design used in the Mars Organic Molecule Analyzer (MOMA) instrument on the 2018 ExoMars rover. LITMS additionally features developments based on the Sample Analysis at Mars (SAM) investigation on MSL and recent NASA-funded prototype efforts in laser mass spectrometry, pyrolysis, and precision subsampling. LITMS brings these combined capabilities to achieve its four measurement objectives: (1) Organics: Broad Survey Detect organic molecules over a wide range of molecular weight, volatility, electronegativity, concentration, and host mineralogy. (2) Organic: Molecular Structure Characterize internal molecular structure to identify individual compounds, and reveal functionalization and processing. (3) Inorganic Host Environment Assess the local chemical

  15. Ion/molecule reactions performed in a miniature cylindrical ion trap mass spectrometer.

    PubMed

    Riter, Leah S; Meurer, Eduardo C; Handberg, Eric S; Laughlin, Brian C; Chen, Hao; Patterson, Garth E; Eberlin, Marcos N; Cooks, R Graham

    2003-09-01

    A recently constructed miniature mass spectrometer, based on a cylindrical ion trap (CIT) mass analyzer, is used to perform ion/molecule reactions in order to improve selectivity for in situ analysis of explosives and chemical warfare agent simulants. Six different reactions are explored, including several of the Eberlin reaction type (M. N. Eberlin and R. G. Cooks, Org. Mass Spectrom., 1993, 28, 679-687) as well as novel gas-phase Meerwein reactions. The reactions include (1) Eberlin transacetalization of the benzoyl, 2,2-dimethyloximinium, and 2,2-dimethylthiooximinium cations with 2,2-dimethyl-1,3-dioxolane to form 2-phenyl-1,3-dioxolanylium cations, 2,2-dimethylamine-1,3-dioxolanylium cations and the 2,2-dimethylamin-1,3-oxathiolanylium cations, respectively; (2) Eberlin reaction of the phosphonium ion CH3P(O)OCH3+, formed from the chemical warfare agent simulant dimethyl methylphosphonate (DMMP), with 1,4-dioxane to yield the 1,3,2-dioxaphospholanium ion, a new characteristic reaction for phosphate ester detection; (3) the novel Meerwein reaction of the ion CH3P(O)OCH3+ with propylene sulfide forming 1,3,2-oxathionylphospholanium ion; (4) the Meerwein reaction of the benzoyl cation with propylene oxide and propylene sulfide to form 4-methyl-2-phenyl-1,3-dioxolane and its thio analog, respectively; (5) ketalization of the benzoyl cation with ethylene glycol to form the 2-phenyl-1,3-dioxolanylium cation; (6) addition/NO2 elimination involving benzonitrile radical cation in reaction with nitrobenzene to form an arylated nitrile, a diagnostic reaction for explosives detection and (7) simple methanol addition to the C7H7+ ion, formed by NO2 loss from the molecular ion of p-nitrotoluene to form an intact adduct. Evidence is provided that these reactions occur to give the products described and their potential analytical utility is discussed. PMID:14529016

  16. Analysis of glycylsarcosine transport by lobster intestine using gas chromatography.

    PubMed

    Peterson, Maria L; Lane, Amy L; Ahearn, Gregory A

    2015-01-01

    Gas chromatography was used to measure transepithelial transport of glycylsarcosine (Gly-Sar) by perfused lobster (Homarus americanus) intestine. Unidirectional and net fluxes of dipeptide across the tissue and luminal factors affecting their magnitude and direction were characterized by perfusing the lumen with the dipeptide and measuring its appearance in saline on the serosal side of the organ. Transmural transport of 10 mM Gly-Sar resulted in serosal accumulation of only the dipeptide; no appearance of corresponding monomeric amino acids glycine or sarcosine was observed. Carrier-mediated and diffusional transmural intestinal transport of Gly-Sar was estimated at 1-15 mM luminal concentrations and followed a curvilinear equation providing a K m = 0.44 ± 0.17 mM, a J max = 1.27 ± 0.12 nmol cm(-2) min(-1), and a diffusional coefficient = 0.026 ± 0.008 nmol cm(-2) min(-1) mM(-1). Unidirectional mucosal to serosal and serosal to mucosal fluxes of 10 mM Gly-Sar provided a significant (p < 0.05) net absorptive flux toward the serosa of 3.54 ± 0.77 nmol cm(-2) min(-1), further supporting carrier-mediated dipeptide transport across the gut. Alkaline (pH 8.5) luminal pH more than doubled transmural Gly-Sar transport as compared to acidic (pH 5.5) luminal pH, while luminal amino acid-metal chelates (e.g., Leu-Zn-Leu), and high concentrations of amino acids alone significantly (p < 0.001) reduced intestinal Gly-Sar transfer by inhibiting carrier transport of the dipeptide. Proposed mechanisms accounting for intestinal dipeptide transport and luminal factors affecting this process are discussed. PMID:25260349

  17. Evaluation of Gas Chromatography/Mini-IMS to Detect VOCs

    NASA Technical Reports Server (NTRS)

    Limero, Thomas; Reese, Eric; Peters, Randy; James, John T.; Billica, Roger (Technical Monitor)

    1999-01-01

    The Toxicology Laboratory at Johnson Space Center (JSC) has pioneered the use of gas chromatography-ion mobility spectrometry (GC/IMS) for measuring target volatile organic compounds (VOCs) aboard spacecraft. Graseby Dynamics, under contract to NASA/Wyle, has built several volatile organic analyzers (VOA) based on GC/IMS. Foremost among these have been the volatile organic analyzer-risk mitigation unit and the two flight VOA units for International Space Station (ISS). The development and evaluation of these instruments has been chronicled through presentations at the International Conference on Ion Mobility Spectrometry over the past three years. As the flight VOA from Graseby is prepared for operation on ISS at JSC, it is time to begin evaluations of technologies for the next generation VOA, Although the desired instrument characteristics for the next generation unit are the same as the current unit, the requirements are much more stringent. As NASA looks toward future missions beyond Earth environs, a premium will be placed upon small, light, reliable, autonomous hardware. It is with these visions in mind that the JSC Toxicology Laboratory began a search for the next generation VOA. One technology that is a candidate for the next generation VOA is GC/IMS. The recent miniaturization of IMS technology permits it to compete with other, inherently small, technologies such as chip-sized sensor arrays. This paper will discuss the lessons learned from the VOA experience and how that has shaped the design of a potential second generation VOA based upon GC/IMS technology. Data will be presented from preliminary evaluations of GC technology and the mini-IMS when exposed to VOCs likely to be detected aboard spacecraft. Results from the evaluation of an integrated GC/mini-IMS system will be shown if available.

  18. [Development of methods for determining acrylamide in food products by gas-liquid chromatography].

    PubMed

    Bessonov, V V; Malinkin, A D; Perederiaev, O I; Bogachuk, M N; Volkovich, S V; Medvedev, Iu V

    2011-01-01

    The method of determination of acrylamide in various food (milk powder, potato chips, instant coffee) by gas-liquid chromatography after pre-bromination was developed. Studies have shown the possibility of using bromination of acrylamide to give it the necessary properties for better extraction, purification and detection. Also revealed the possibility of qualitative and quantitative determine a acrylamide in food by gas-liquid chromatography with detection by electron capture detector. PMID:22232888

  19. Initial commissioning results with the NSCL Electron Beam Ion Trap

    SciTech Connect

    Schwarz, S.; Kittimanapun, K.; Lapierre, A.; Leitner, D.; Ottarson, J.; Portillo, M.; Bollen, G.; Lopez-Urrutia, J. R. Crespo; Kester, O.

    2012-02-15

    The ReA reaccelerator is being added to the National Superconducting Cyclotron Laboratory (NSCL) fragmentation facility in order to provide exotic rare-isotope beams, not available at the Isotope Separation On-Line facilities, in the several-MeV/u energy range. The first stage of the NSCL reaccelerator complex, consisting of an EBIT charge breeder, a room-temperature radiofrequency quadrupole (RFQ) accelerator, and superconducting linear accelerator modules, has been completed and is being put into operation. Commissioning of the EBIT has started by extracting charge-bred residual gas ions, ions created from a Ne gas jet directed across the EBIT's electron beam and ions captured from an external test ion source. Charge-bred ions from the Ne gas jet have been extracted as a pulse and accelerated through the RFQ and the two cryomodules.

  20. DIRECT TRACE ANALYSIS OF VOLATILE ORGANIC COMPOUNDS IN AIR USING ION TRAP MASS SPECTROMETERS WITH FILTERED NOISE FIELDS

    EPA Science Inventory

    Two ion trap mass spectrometers and direct air sampling interfaces are being evaluated in the laboratory for monitoring toxic air pollutants in real time. he mass spectrometers are the large, laboratory-based Finnigan MAT ion trap (ITMS) and the compact, field-deployable Teledyne...

  1. Analysis of pesticide residues in tobacco with online size exclusion chromatography with gas chromatography and tandem mass spectrometry.

    PubMed

    Guo, Weiyun; Bian, Zhaoyang; Tang, Gangling; Wang, Deguo; Li, Guanghui; Wang, Jianlong

    2016-07-01

    An ultrasensitive method for the simultaneous analysis of pesticides residues in tobacco was developed with online size exclusion chromatography with gas chromatography and tandem mass spectrometry. Tobacco samples were extracted with the solvent mixture of cyclohexane and acetone (7:3, v/v) and centrifuged. Then, the supernatant liquors were injected directly into the online size exclusion chromatography with gas chromatography and tandem mass spectrometry without any other purification procedures after being filtered with a 0.22 μm organic phase filter. The matrix interferences were effectively removed and recoveries of most pesticides were in the range of 72-121%. Especially, for chlorothalonil, the analysis efficiency of this method was much more favorable than that of the general method, in which dispersive solid-phase extraction was used as an additional purified procedure. In addition, the limits of quantitation of this method were from 1 to 50 μg/kg. Therefore, a rapid, cost-effective, labor-saving method was proposed in the present work, which was suitable for the analysis of 41 pesticide residues in tobacco. PMID:27197809

  2. X-ray spectroscopy of highly-ionized atoms in an electron beam ion trap (EBIT)

    SciTech Connect

    Marrs, R.E.; Bennett, C.; Chen, M.H.; Cowan, T.; Dietrich, D.; Henderson, J.R.; Knapp, D.A.; Levine, M.A.; Schneider, M.B.; Scofield, J.H.

    1988-01-01

    An Electron Beam Ion Trap at Lawrence Livermore National Laboratory is being used to produce and trap very-highly-charged-ions (q /le/ 70+) for x-ray spectroscopy measurements. Recent measurements of dielectronic recombination, electron impact excitation and transition energies are presented. 15 refs., 12 figs., 1 tab.

  3. The JPL Hg(sup +) Extended Linear Ion Trap Frequency Standard: Status, Stability, and Accuracy Prospects

    NASA Technical Reports Server (NTRS)

    Tjoelker, R. L.; Prestage, J. D.; Maleki, L.

    1996-01-01

    Microwave frequency standards based on room temperature (sup 199)Hg(sup +) ions in a Linear Ion Trap (LITS) presently achieve a Signal to Noise and line Q inferred short frequency stability. Long term stability has been measured for averaging intervals up to 5 months with apparent sensitivity to variations in ion number/temperature limiting the flicker floor.

  4. Advanced Automation for Ion Trap Mass Spectrometry-New Opportunities for Real-Time Autonomous Analysis

    NASA Technical Reports Server (NTRS)

    Palmer, Peter T.; Wong, C. M.; Salmonson, J. D.; Yost, R. A.; Griffin, T. P.; Yates, N. A.; Lawless, James G. (Technical Monitor)

    1994-01-01

    The utility of MS/MS for both target compound analysis and the structure elucidation of unknowns has been described in a number of references. A broader acceptance of this technique has not yet been realized as it requires large, complex, and costly instrumentation which has not been competitive with more conventional techniques. Recent advancements in ion trap mass spectrometry promise to change this situation. Although the ion trap's small size, sensitivity, and ability to perform multiple stages of mass spectrometry have made it eminently suitable for on-line, real-time monitoring applications, advance automation techniques are required to make these capabilities more accessible to non-experts. Towards this end we have developed custom software for the design and implementation of MS/MS experiments. This software allows the user to take full advantage of the ion trap's versatility with respect to ionization techniques, scan proxies, and ion accumulation/ejection methods. Additionally, expert system software has been developed for autonomous target compound analysis. This software has been linked to ion trap control software and a commercial data system to bring all of the steps in the analysis cycle under control of the expert system. These software development efforts and their utilization for a number of trace analysis applications will be described.

  5. [Analysis of cracking gas compressor fouling by pyrolysis gas chromatography-mass spectrometry].

    PubMed

    Hu, Yunfeng; Fang, Fei; Wei, Tao; Liu, Shuqing; Jiang, Guangshen; Cai, Jun

    2013-06-01

    The fouling from the different sections of the cracked gas compressor in Daqing Petrochemical Corporation was analyzed by pyrolysis gas chromatography-mass spectrometry (Py/GC-MS). All the samples were cracked in RJ-1 tube furnace cracker at the cracking temperature of 500 degrees C, and separated with a 60 m DB-1 capillary column. An electron impact ionization (EI) source was used with the ionizing voltage of 70 eV. The results showed the formation of fouling was closely related with cyclopentadiene which accounted for about 50% of the cracking products. Other components detected were 1-butylene, propylene, methane and n-butane. This Py/GC-MS method can be used as an effective approach to analyze the causes of fouling in the petrochemical plants. PMID:24063202

  6. Chromatography

    MedlinePlus

    ... a way of separating two or more chemical compounds. Chemical compounds are chemicals that are bonded together. For example, ... and hydrogen. Proteins are another type of chemical compound. There are different kinds of chromatography. These include ...

  7. Pressurised hot water extraction followed by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry for the determination of N-nitrosamines in sewage sludge.

    PubMed

    Llop, Anna; Borrull, Francesc; Pocurull, Eva

    2012-01-15

    A method for the quantitative determination of the nine EPA N-nitrosamines in sewage sludge was developed by using pressurised hot water extraction (PHWE) followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to chemical ionization ion trap tandem mass spectrometry (GC-CI-MS-MS). The pressurised hot water extraction was optimized using a central composite design with regard to operational parameters such as temperature, extraction time and pH of water as extracting solvent. The optimum conditions were: water at pH 7.5 as extracting solvent, temperature of 125°C and extraction time of 5 min. The sewage sludge extract was automatically analyzed by HS-SPME using a divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber and GC-CI-MS-MS. The limits of detection of all compounds were lower than 0.15 μg/kg of dry weight (d.w.) of sewage sludge. The repeatability and reproducibility between days (10μg/kg d.w.) expressed as relative standard deviation were lower than 16 and 19%, respectively. The method was applied to determine the N-nitrosamines in sewage sludge from urban and industrial sewage treatment plants (STPs) and from a potable water treatment plant. Some N-nitrosamines were determined in the samples and N-nitrosodiethylamine (NDEA) and N-nitrosodi-n-butylamine (NDBA) showed the highest values (371 and 305 μg/kg (d.w.), respectively) in sewage from industrial STPs. PMID:22265500

  8. Final Report - Advanced Ion Trap Mass Spectrometry Program - Oak Ridge National Laboratory - Sandia National Laboratory

    SciTech Connect

    Whitten, W.B.

    2002-12-18

    This report covers the three main projects that collectively comprised the Advanced Ion Trap Mass Spectrometry Program. Chapter 1 describes the direct interrogation of individual particles by laser desorption within the ion trap mass spectrometer analyzer. The goals were (1) to develop an ''intelligent trigger'' capable of distinguishing particles of biological origin from those of nonbiological origin in the background and interferent particles and (2) to explore the capability for individual particle identification. Direct interrogation of particles by laser ablation and ion trap mass spectrometry was shown to have good promise for discriminating between particles of biological origin and those of nonbiological origin, although detailed protocols and operating conditions were not worked out. A library of more than 20,000 spectra of various types of biological particles has been assembled. Methods based on multivariate analysis and on neural networks were used to discriminate between particles of biological origin and those of nonbiological origin. It was possible to discriminate between at least some species of bacteria if mass spectra of several hundred similar particles were obtained. Chapter 2 addresses the development of a new ion trap mass analyzer geometry that offers the potential for a significant increase in ion storage capacity for a given set of analyzer operating conditions. This geometry may lead to the development of smaller, lower-power field-portable ion trap mass spectrometers while retaining laboratory-scale analytical performance. A novel ion trap mass spectrometer based on toroidal ion storage geometry has been developed. The analyzer geometry is based on the edge rotation of a quadrupolar ion trap cross section into the shape of a torus. Initial performance of this device was poor, however, due to the significant contribution of nonlinear fields introduced by the rotation of the symmetric ion-trapping geometry. These nonlinear resonances

  9. PROGRAM DOCUMENTATION FOR THE GAS CHROMATOGRAPHY AUTOMATION SYSTEM

    EPA Science Inventory

    This documentation contains the program listings, program flowcharts, symbol definitions, symbol references, and program descriptions of all the BASIC language programs which implement the functional specifications for an advanced chromatography automation system (EPA report PB80...

  10. Structure elucidation of degradation products of the antibiotic amoxicillin with ion trap MS(n) and accurate mass determination by ESI TOF.

    PubMed

    Nägele, Edgar; Moritz, Ralf

    2005-10-01

    Today, it is necessary to identify relevant compounds appearing in discovery and development of new drug substances in the pharmaceutical industry. For that purpose, the measurement of accurate molecular mass and empirical formula calculation is very important for structure elucidation in addition to other available analytical methods. In this work, the identification and confirmation of degradation products in a finished dosage form of the antibiotic drug amoxicillin obtained under stress conditions will be demonstrated. Structure elucidation is performed utilizing liquid chromatography (LC) ion trap MS/MS and MS3 together with accurate mass measurement of the molecular ions and of the collision induced dissociation (CID) fragments by liquid chromatography electro spray ionization time-of-flight mass spectrometry (LC/ESI-TOF). PMID:16099170

  11. DETERMINATION OF ORGANOTINS IN WATER BY MICRO-LIQUID CHROMATOGRAPHY-ELECTROSPRAY ION TRAP MASS SPECTROMETRY

    EPA Science Inventory

    Due to the varying toxicity the species of organotins in their widespread applications, it is important for analytical methods to address their speciation. Traditional methods call for the hydrolysis and subsequent derivatization of the organotins before analysis. These methods...

  12. ANALYSIS OF AMBIENT POLAR VOLATILE ORGANIC COMPOUNDS USING CHEMICAL IONIZATION -- ION TRAP DETECTOR

    EPA Science Inventory

    The current approach to measuring trace levels of volatile organic compounds (VOCs) in ambient air requires cryogenic trapping of the analytes, followed by thermal desorption and low-temperature refocussing onto a column for analysis by capillary gas chromatography/mass spectrome...

  13. Surface characterization of industrial fibers with inverse gas chromatography.

    PubMed

    van Asten, A; van Veenendaal, N; Koster, S

    2000-08-01

    Inverse gas chromatography (IGC) was applied for the determination of the surface characteristics of Tenax carbon fibers and Akzo Nobel Twaron fibers. Furthermore, IGC procedures for the determination of dispersive and acid-base interactions were validated. The data show that too high values for the dispersive component of the surface energy are obtained when the adsorption area occupied by a single adsorbed n-alkane molecule is estimated from parameters of the corresponding liquid. Comparable values are obtained when the Doris-Gray methodology (area per methylene unit) or measured probe areas are employed. For the fibers studied in this work meaningful Gibbs energy values of the acid-base interaction were only obtained with the polarizability approach. When the dispersive interaction of the polar probes with the fiber surface was scaled to the n-alkane interaction via surface tension, the boiling point, or the vapor pressure of the probes often negative acid-base interaction energies were found. From the temperature dependence of the Gibbs energy, the enthalpy of the acid-base interactions of various probes with the carbon and Twaron aramid fibers was determined. However, from these enthalpy values no meaningful acid-base surface parameters could be obtained. Generally, the limited accuracy with which these parameters can be obtained make the usefulness of this procedure questionable. Also the Gibbs energy data of acid-base interaction can provide a qualitative basis to classify the acidity-basicity of the fiber surface. This latter approach requires only a limited data set and is sufficiently rapid to enable the use of IGC as a screening tool for fibers at a production site. For several polar probes significant concentration effects on carbon fibers were observed. At very low probe loadings the interaction with the fiber surface suddenly increases. This effect is caused by the heterogeneity of the interaction energy of the active sites at the surface. A simple

  14. High resolution gas chromatography analysis of rice bran oil

    NASA Astrophysics Data System (ADS)

    Yu, Fengxiang; Lin, Qinlu; Chen, Xu; Wei, Xiaojun

    To assess the nutritional value and safety quality of rice bran oil (RBO) ,fatty acids of RBO from 15 species rice come from Hunan Province were analyzed by high resolution gas chromatography (HRGC). Crude RBOs were extracted by hexane 3-times using a solvent-to-rice bran ratio of 3:1 (w/w) at 40°C and composition of RBOs was analyzed by HRGC. The result showed that main fatty acids of 15 kinds of RBO include myristic acid (C14:0), palmitic acid (C16:0), palmitoleic acid (C16:1), stearic acid (C18:0), oleic acid (C18:1), linoleic acid (C18:2), linolenic acid (C18:3), arachidic acid (C20:0), arachidonic acid (C20:1). It is strange that arachidonic acid (C20:1) is not listed in Chinese standard of RBO (GB11192-2003), and it exists in our samples of RBO. The average value of linolenic acid in RBOs is 1.6304% (range from 1.2425% to 2.131%), and it showed higher level comparing with Chinese standard that linolenic acid is less than 1.0%. The average value of USFA and SFA are 76.81% (range 75.96% to 82.06% ) and 20.15% (range 13.72% to 23.06%) respectively, and USFA content is close to olive oil (83.75%), peanut oil (81.75%) and soybean oil (85.86%). USFA in Jingyou 13 RBO is the highest content. The ratio of USFA to SFA content is 4:1 (range from 3.32 to 5.98:1). The ratio of SFA: MUFA: PUFA of 15 RBOs is 1: 2.2: 1.8, and ω6/ω3 ratio is 21.69 (range from16.54 to 27.28) and it is close to the 26:1 which is reported to be helpful to increase SOD activity. The oleic acid /linoleic acid ratio of 15 RBOs is 1.23:1 (rang from 1.04:1 to 1.42:1). Our data analyzed composition of RBOs from 15 species rice of China and will provide new evidence to revise RBO standard. It also helps us to assess nutritional value of RBOs and identify different RBOs from various species rice and places of origin.

  15. Gold Nanoparticle Chemiresistor Arrays for Micro-Gas Chromatography Applications

    NASA Astrophysics Data System (ADS)

    Covington, Elizabeth Laura

    Thiolate-monolayer-protected gold nanoparticle (MPN) chemiresistors were studied as the sensing devices for micro-gas chromatography (microGC) systems. Because transport through chemiresistors is dominated by tunneling, they are highly sensitive. In order to improve their limit of detection, their fundamental noise was studied. Chemiresistors exhibit 1/f type noise where noise scales inversely with frequency. Chemiresistor noise was found to scale inversely with MPN film thickness. We lowered the noise prefactor of a 50x60 microm2 chemiresistor by coating a thick rather than monolayer MPN film. Electron beam induced crosslinking (EBIX) of the MPN film slightly reduced chemiresistor noise. A technique for patterning chemiresistor arrays with MPN films using EBIX was developed, and an array with four distinct MPNs was fabricated in an area ˜600 microm 2. This is the smallest chemiresistor array reported to date. Chemiresistors were exposed to vapors and provided differential sensitivities comparable to those from larger uncrosslinked chemiresistors. Chemiresistors were studied to assess their long term stability. Chemiresistors exhibited decreases in resistance over time that is likely caused by loss of MPN ligands. Temperature dependent current-voltage measurements verified the resistance change was not due to changes in the size of the MPN core. While resistance could change by orders of magnitude, vapor sensitivity did not show significant changes. Heating increased the change in resistance, but chemiresistors remained responsive after being held at 80°C for a cumulative 400 hours. It was unknown whether tunneling in the MPN film is through the highest unoccupied molecular orbital (HOMO) or lowest unoccupied molecular orbital (LUMO). A new technique was explored to distinguish tunneling through the HOMO and LUMO by measuring the induced thermoelectric voltage caused by a temperature difference across the MPN film. For integration into a microGC system, we

  16. The use of a milli-whistle as a detector in gas analysis by gas chromatography.

    PubMed

    Lin, Cheng-Huang; He, Yi-San; Lin, Chien-Hung; Fan, Gang-Ting; Chen, Hsin-Kai

    2014-01-01

    This mini-review introduces a general understanding of the use of a milli-whistle as a gas chromatography (GC) detector in gas analysis, including our research on the methodology and theory associated with a number of different related applications. The milli-whistle is connected to the outlet of a GC capillary, and when the eluted gases and the GC carrier gas pass through it, a sound with a fundamental frequency is produced. The sound wave can be picked up by a microphone or an accelerometer, and after a fast Fourier transform, the online data obtained for frequency-change vs. retention time constitute a new method for detecting gases. The first part of this review discusses the fundamentals of the milli-whistle. Some modifications are also discussed, including various types of whistles and an attempt to maximize the sensitivity and stability of the method. The second part then focuses on several practical applications, including an analysis of hydrogen released from ammonia borane, inorganic gases produced from fireworks, the CO2/O2 ratio from expired human breath and a purity test for alcohols. These studies show that the GC-whistle method has great potential for use as a fast sampling ionization method, and for the direct analysis of biological and chemical samples at under ambient conditions. PMID:24420261

  17. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    USGS Publications Warehouse

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  18. Identification of cephapirin metabolites and degradants in bovine milk by electrospray ionization--ion trap tandem mass spectrometry.

    PubMed

    Heller, D N; Kaplan, D A; Rummel, N G; von Bredow, J

    2000-12-01

    Liquid chromatography-ion trap tandem mass spectrometry (LC-MS/MS) with electrospray ionization was used to identify cephapirin metabolites and degradants in milk from cows dosed with cephapirin. The milk was extracted according to a previously published procedure. Structures for various components were tentatively identified by their molecular weight, product ion mass spectra, and/or correspondence to standard mass spectra. These components may have occurred as metabolites or as degradants that occurred on storage or during extraction. Compounds identified in the milk included cephapirin, desacetylcephapirin, cephapirin lactone, hydrolyzed cephapirin, and a reduced cephapirin lactone that has not previously been reported. Methylcephapirin was also identified, possibly as a trace contaminant in the formulation. Analysis of incurred milk extracts showed that cephapirin and desacetylcephapirin are the major residues in milk. Desacetylcephapirin residues persisted about as long as the parent drug. The detection limit for both residues by LC-MS/MS was approximately 1 ng/mL in milk. These results have implications for microbiological methods or rapid test kits, if such methods or kits respond to cephapirin metabolites and degradants present in the milk. PMID:11141270

  19. Analysis of methaqualone in biological matrices by micellar electrokinetic capillary chromatography. Comparison with gas chromatography-mass spectrometry.

    PubMed

    Plaut, O; Girod, C; Staub, C

    1998-04-01

    The analysis of methaqualone (MTQ) in biological matrices by capillary electrophoresis (CE) is described. This methods uses liquid-liquid extraction and micellar electrokinetic capillary chromatography (MECC), an operation mode of CE. Separations are made using a 25 cm long capillary and a borate/phosphate buffer at pH 8.2. Using gas chromatography with mass spectrometry detection (GC-MS) as reference method, MTQ has been analyzed in urine, blood, gastric content and hair. For hair analysis, supercritical fluid extraction was compared with liquid-liquid extraction. Linearity was established in urine and blood between 0.25 and 10.0 micrograms/ml. MTQ recovery from blood was estimated at 60%. The limit of detection of this method in urine is about 0.10 microgram/ml. Drawbacks and advantages of MECC over GC-MS are discussed. PMID:9627981

  20. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    SciTech Connect

    C.J. Miller; G. Elias; N.C. Schmitt; C. Rae

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to specifically identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol using no sample cleanup prior to analysis. The methanol extracts were injected directly into several different column types and analyzed by HPLC-UV and/or GC-ECD. This paper describes general screening methods that were used to determine the presence of explosives in unknown samples and techniques that have been optimized for quantification of each explosive from the substrate extracts.

  1. Community air monitoring for pesticides-part 2: multiresidue determination of pesticides in air by gas chromatography, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry.

    PubMed

    Hengel, Matt; Lee, P

    2014-03-01

    Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography-mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37-104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70-170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air. PMID:24370860

  2. Note: A novel design of a microwave feed for a microwave frequency standard with a linear ion trap

    SciTech Connect

    Zhang, J. W. Miao, K.; Wang, S. G.; Wang, Z. B.

    2014-07-15

    Linear ion traps are important tools in many applications, particularly in mass spectrum analyzers and frequency standards. Here a novel design of a microwave feed integrated into one electrode of a linear quadrupole ion trap is demonstrated for the application of a microwave frequency standard based on cadmium ions. The mechanical structure of the microwave feed is compact and easy to build. The ion trap integrated with this microwave feed is successfully applied to measure the hyperfine splitting of the ground state of {sup 113}Cd{sup +}, thus demonstrating the practicality and reliability of the microwave feed.

  3. Using metal complex ion-molecule reactions in a miniature rectilinear ion trap mass spectrometer to detect chemical warfare agents.

    PubMed

    Graichen, Adam M; Vachet, Richard W

    2013-06-01

    The gas-phase reactions of a series of coordinatively unsaturated [Ni(L)n](y+) complexes, where L is a nitrogen-containing ligand, with chemical warfare agent (CWA) simulants in a miniature rectilinear ion trap mass spectrometer were investigated as part of a new approach to detect CWAs. Results show that upon entering the vacuum system via a poly(dimethylsiloxane) (PDMS) membrane introduction, low concentrations of several CWA simulants, including dipropyl sulfide (simulant for mustard gas), acetonitrile (simulant for the nerve agent tabun), and diethyl phosphite (simulant for nerve agents sarin, soman, tabun, and VX), can react with metal complex ions generated by electrospray ionization (ESI), thereby providing a sensitive means of detecting these compounds. The [Ni(L)n](2+) complexes are found to be particularly reactive with the simulants of mustard gas and tabun, allowing their detection at low parts-per-billion (ppb) levels. These detection limits are well below reported exposure limits for these CWAs, which indicates the applicability of this new approach, and are about two orders of magnitude lower than electron ionization detection limits on the same mass spectrometer. The use of coordinatively unsaturated metal complexes as reagent ions offers the possibility of further tuning the ion-molecule chemistry so that desired compounds can be detected selectively or at even lower concentrations. PMID:23532782

  4. Using Metal Complex Ion-Molecule Reactions in a Miniature Rectilinear Ion Trap Mass Spectrometer to Detect Chemical Warfare Agents

    NASA Astrophysics Data System (ADS)

    Graichen, Adam M.; Vachet, Richard W.

    2013-06-01

    The gas-phase reactions of a series of coordinatively unsaturated [Ni(L)n]y+ complexes, where L is a nitrogen-containing ligand, with chemical warfare agent (CWA) simulants in a miniature rectilinear ion trap mass spectrometer were investigated as part of a new approach to detect CWAs. Results show that upon entering the vacuum system via a poly(dimethylsiloxane) (PDMS) membrane introduction, low concentrations of several CWA simulants, including dipropyl sulfide (simulant for mustard gas), acetonitrile (simulant for the nerve agent tabun), and diethyl phosphite (simulant for nerve agents sarin, soman, tabun, and VX), can react with metal complex ions generated by electrospray ionization (ESI), thereby providing a sensitive means of detecting these compounds. The [Ni(L)n]2+ complexes are found to be particularly reactive with the simulants of mustard gas and tabun, allowing their detection at low parts-per-billion (ppb) levels. These detection limits are well below reported exposure limits for these CWAs, which indicates the applicability of this new approach, and are about two orders of magnitude lower than electron ionization detection limits on the same mass spectrometer. The use of coordinatively unsaturated metal complexes as reagent ions offers the possibility of further tuning the ion-molecule chemistry so that desired compounds can be detected selectively or at even lower concentrations.

  5. Plug-and-Play Planar Ion Traps for Scalable Quantum Computation and Simulation

    NASA Astrophysics Data System (ADS)

    Amini, Jason; Denison, Douglas; Doret, S. Charles; Faircloth, Daniel; Hayden, Harley; Killian, Tyler; Landgren, David; Martin, Kevin; Merrill, True; Ozakin, Arkadas; Pai, C. S.; Shaikh, Fayaz; Shappert, Chris; Volin, Curtis; Wright, Ken; Harter, Alexa; Slusher, Richart

    2011-05-01

    At the heart of most ion-based quantum information processing and simulation efforts is an RF-Paul trap to confine the ion qubits. Cutting edge experiments are transitioning from a few qubits to a few tens of qubits with many more qubits envisioned for the future. The underlying ion traps need to both grow with the experiments and provide additional features that can simplify and extend these experiments. The Georgia Tech Research Institute (GTRI) is developing modeling and fabrication processes for these new generations of ion traps using silicon VLSI technology in surface- electrode geometries. Verified by detailed in-house trap characterization, GTRI has fabricated traps that approach the plug- and-play ideal and demonstrate reliable ion loading and transport, long dark lifetimes, and stable ion chains. Additional features are in development including junctions, integrated GHz range current guides for global qubit rotations, and micromirrors for light collection.

  6. High Energy Laboratory Astrophysics Experiments using electron beam ion traps and advanced light sources

    NASA Astrophysics Data System (ADS)

    Brown, Gregory V.; Beiersdorfer, Peter; Bernitt, Sven; Eberle, Sita; Hell, Natalie; Kilbourne, Caroline; Kelley, Rich; Leutenegger, Maurice; Porter, F. Scott; Rudolph, Jan; Steinbrugge, Rene; Traebert, Elmar; Crespo-Lopez-Urritia, Jose R.

    2015-08-01

    We have used the Lawrence Livermore National Laboratory's EBIT-I electron beam ion trap coupled with a NASA/GSFC microcalorimeter spectrometer instrument to systematically address problems found in the analysis of high resolution X-ray spectra from celestial sources, and to benchmark atomic physics codes employed by high resolution spectral modeling packages. Our results include laboratory measurements of transition energies, absolute and relative electron impact excitation cross sections, charge exchange cross sections, and dielectronic recombination resonance strengths. More recently, we have coupled to the Max-Plank Institute for Nuclear Physics-Heidelberg's FLASH-EBIT electron beam ion trap to third and fourth generation advanced light sources to measure photoexcitation and photoionization cross sections, as well as, natural line widths of X-ray transitions in highly charged iron ions. Selected results will be presented.

  7. Compact soft x-ray spectrometer for plasma diagnostics at the Heidelberg Electron Beam Ion Trap

    SciTech Connect

    Lapierre, A.; Crespo Lopez-Urrutia, J. R.; Baumann, T. M.; Epp, S. W.; Gonchar, A.; Gonzalez Martinez, A. J.; Liang, G.; Rohr, A.; Soria Orts, R.; Simon, M. C.; Tawara, H.; Versteegen, R.; Ullrich, J.

    2007-12-15

    A compact flat-field soft x-ray grazing-incidence grating spectrometer equipped with a cryogenically cooled back-illuminated charge-coupled device camera was built and implemented at the Heidelberg Electron Beam Ion Trap. The instrument spans the spectral region from 1 to 37 nm using two different gratings. In slitless operation mode, it directly images a radiation source, in this case ions confined in an electron beam ion trap, with high efficiency and reaching hereby a resolving power of {lambda}/{delta}{lambda} congruent with 130 at 2 nm and of {lambda}/{delta}{lambda} congruent with 600 at 28 nm. Capable of automatized operation, its low noise and excellent stability make it an ideal instrument not only for spectroscopic diagnostics requiring wide spectral coverage but also for precision wavelength measurements.

  8. Operation of a planar-electrode ion-trap array with adjustable RF electrodes

    NASA Astrophysics Data System (ADS)

    Kumph, M.; Holz, P.; Langer, K.; Meraner, M.; Niedermayr, M.; Brownnutt, M.; Blatt, R.

    2016-02-01

    One path to realizing systems of trapped atomic ions suitable for large-scale quantum computing and simulation is to create a two-dimensional (2D) array of ion traps. Interactions between nearest-neighbouring ions could then be turned on and off by tuning the ions’ relative positions and frequencies. We demonstrate and characterize the operation of a planar-electrode ion-trap array. By driving the trap with a network of phase-locked radio-frequency resonators which provide independently variable voltage amplitudes we vary the position and motional frequency of a Ca+ ion in two-dimensions within the trap array. Work on fabricating a miniaturised form of this 2D trap array is also described, which could ultimately provide a viable architecture for large-scale quantum simulations.

  9. Human Biomonitoring of DNA Adducts by Ion Trap Multistage Mass Spectrometry.

    PubMed

    Guo, Jingshu; Turesky, Robert J

    2016-01-01

    Humans are continuously exposed to hazardous chemicals in the environment. These chemicals or their electrophilic metabolites can form adducts with genomic DNA, which can lead to mutations and the initiation of cancer. The identification of DNA adducts is required for understanding exposure and the etiological role of a genotoxic chemical in cancer risk. The analytical chemist is confronted with a great challenge because the levels of DNA adducts generally occur at <1 adduct per 10(7) nucleotides, and the amount of tissue available for measurement is limited. Ion trap mass spectrometry has emerged as an important technique to screen for DNA adducts because of the high level sensitivity and selectivity, particularly when employing multi-stage scanning (MS(n) ). The product ion spectra provide rich structural information and corroborate the adduct identities even at trace levels in human tissues. Ion trap technology represents a significant advance in measuring DNA adducts in humans. © 2016 by John Wiley & Sons, Inc. PMID:27584705

  10. Ion Trapping, Storage, and Ejection in Structures for Lossless Ion Manipulations

    SciTech Connect

    Zhang, Xinyu; Garimella, Venkata BS; Prost, Spencer A.; Webb, Ian K.; Chen, Tsung-Chi; Tang, Keqi; Tolmachev, Aleksey V.; Norheim, Randolph V.; Baker, Erin Shammel; Anderson, Gordon A.; Ibrahim, Yehia M.; Smith, Richard D.

    2015-06-16

    A structure for lossless ion manipulation (SLIM) module was constructed with electrode arrays patterned on a pair of parallel printed circuit boards (PCB) separated by 5 mm and utilized to investigate capabilities for ion trapping at 4 Torr. Positive ions were confined by application of RF having alternating phases on a series of inner rung electrodes and by positive DC potentials on surrounding guard electrodes on each PCB. An axial DC field was also introduced by stepwise varying the DC potential of the inner rung electrodes so as to control the ion transport and accumulation inside the ion trap. We show that ions could be trapped and accumulated with 100% efficiency, stored for at least 5 hours with no losses, and could be rapidly ejected from the SLIM trap.

  11. Low power high-performance radio frequency oscillator for driving ion traps

    SciTech Connect

    Jau, Y.-Y.; Benito, F. M.; Partner, H.; Schwindt, P. D. D.

    2011-02-15

    We report a simple, efficient, high voltage radio frequency (RF) generator powered by a single voltage source (1.5-7 V) to resonantly drive ion traps or other capacitive loads. Our circuit is able to deliver RF voltages > 500 V{sub p-p} at frequencies ranging from 0.1 to 10 MHz. This RF oscillator uses low-cost, commercially available components, and can be easily assembled onto a circuit board of a few cm{sup 2}. Because of its simplicity and good efficiency, this circuit is useful in applications requiring small size and low power consumption such as portable ion trap systems where the duration of operation under battery power is of concern.

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

    SciTech Connect

    Thompson, Cyril V.; Whitten, William B.

    2015-11-01

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

  13. Electronics of an ion trap with integrated time-of-flight mass spectrometer

    NASA Astrophysics Data System (ADS)

    Schneider, Christian; Schowalter, Steven J.; Yu, Peter; Hudson, Eric R.

    2016-01-01

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

  14. Ion Trapping, Storage, and Ejection in Structures for Lossless Ion Manipulations.

    PubMed

    Zhang, Xinyu; Garimella, Sandilya V B; Prost, Spencer A; Webb, Ian K; Chen, Tsung-Chi; Tang, Keqi; Tolmachev, Aleksey V; Norheim, Randolph V; Baker, Erin S; Anderson, Gordon A; Ibrahim, Yehia M; Smith, Richard D

    2015-06-16

    A new Structures for Lossless Ion Manipulations (SLIM) module, having electrode arrays patterned on a pair of parallel printed circuit boards (PCB), was constructed and utilized to investigate capabilities for ion trapping at a pressure of 4 Torr. Positive ions were confined by application of RF voltages to a series of inner rung electrodes with alternating phase on adjacent electrodes, in conjunction with positive DC potentials on surrounding guard electrodes on each PCB. An axial DC field was also introduced by stepwise varying the DC potentials applied to the inner rung electrodes to control the ion transport and accumulation inside the ion trapping region. We show that ions can be trapped and accumulated with up to 100% efficiency, stored for at least 5 h with no significant losses, and then could be rapidly ejected from the SLIM trap. The present results provide a foundation for the development of much more complex SLIM devices that facilitate extended ion manipulations. PMID:25971536

  15. Experimental Characterization of Secular Frequency Scanning in Ion Trap Mass Spectrometers

    NASA Astrophysics Data System (ADS)

    Snyder, Dalton T.; Pulliam, Christopher J.; Wiley, Joshua S.; Duncan, Jason; Cooks, R. Graham

    2016-07-01

    Secular frequency scanning is implemented and characterized using both a benchtop linear ion trap and a miniature rectilinear ion trap mass spectrometer. Separation of tetraalkylammonium ions and those from a mass calibration mixture and from a pesticide mixture is demonstrated with peak widths approaching unit resolution for optimized conditions using the benchtop ion trap. The effects on the spectra of ion trap operating parameters, including waveform amplitude, scan direction, scan rate, and pressure are explored, and peaks at black holes corresponding to nonlinear (higher-order field) resonance points are investigated. Reverse frequency sweeps (increasing mass) on the Mini 12 are shown to result in significantly higher ion ejection efficiency and superior resolution than forward frequency sweeps that decrement mass. This result is accounted for by the asymmetry in ion energy absorption profiles as a function of AC frequency and the shift in ion secular frequency at higher amplitudes in the trap due to higher order fields. We also found that use of higher AC amplitudes in forward frequency sweeps biases ions toward ejection at points of higher order parametric resonance, despite using only dipolar excitation. Higher AC amplitudes also increase peak width and decrease sensitivity in both forward and reverse frequency sweeps. Higher sensitivity and resolution were obtained at higher trap pressures in the secular frequency scan, in contrast to conventional resonance ejection scans, which showed the opposite trend in resolution on the Mini 12. Mass range is shown to be naturally extended in secular frequency scanning when ejecting ions by sweeping the AC waveform through low frequencies, a method which is similar, but arguably superior, to the more usual method of mass range extension using low q resonance ejection.

  16. Comparison of Data Acquisition Strategies on Quadrupole Ion Trap Instrumentation for Shotgun Proteomics

    NASA Astrophysics Data System (ADS)

    Canterbury, Jesse D.; Merrihew, Gennifer E.; MacCoss, Michael J.; Goodlett, David R.; Shaffer, Scott A.

    2014-12-01

    The most common data collection in shotgun proteomics is via data-dependent acquisition (DDA), a process driven by an automated instrument control routine that directs MS/MS acquisition from the highest abundant signals to the lowest. An alternative to DDA is data-independent acquisition (DIA), a process in which a specified range in m/ z is fragmented without regard to prioritization of a precursor ion or its relative abundance in the mass spectrum, thus potentially offering a more comprehensive analysis of peptides than DDA. In this work, we evaluate both DDA and DIA on three different linear ion trap instruments: an LTQ, an LTQ modified with an electrodynamic ion funnel, and an LTQ Velos. These instruments represent both older (LTQ) and newer (LTQ Velos) ion trap designs (i.e., linear versus dual ion traps, respectively), and allow direct comparison of peptide identifications using both DDA and DIA analysis. Further, as the LTQ Velos has an enhanced "S-lens" ion guide to improve ion flux, we found it logical to determine if the former LTQ model could be leveraged by improving sensitivity by modifying with an electrodynamic ion guide of significantly different design to the S-lens. We find that the ion funnel enabled LTQ identifies more proteins in the insoluble fraction of a yeast lysate than the other two instruments in DIA mode, whereas the faster scanning LTQ Velos performs better in DDA mode. We explore reasons for these results, including differences in scan speed, source ion optics, and linear ion trap design.

  17. Experimental Characterization of Secular Frequency Scanning in Ion Trap Mass Spectrometers

    NASA Astrophysics Data System (ADS)

    Snyder, Dalton T.; Pulliam, Christopher J.; Wiley, Joshua S.; Duncan, Jason; Cooks, R. Graham

    2016-03-01

    Secular frequency scanning is implemented and characterized using both a benchtop linear ion trap and a miniature rectilinear ion trap mass spectrometer. Separation of tetraalkylammonium ions and those from a mass calibration mixture and from a pesticide mixture is demonstrated with peak widths approaching unit resolution for optimized conditions using the benchtop ion trap. The effects on the spectra of ion trap operating parameters, including waveform amplitude, scan direction, scan rate, and pressure are explored, and peaks at black holes corresponding to nonlinear (higher-order field) resonance points are investigated. Reverse frequency sweeps (increasing mass) on the Mini 12 are shown to result in significantly higher ion ejection efficiency and superior resolution than forward frequency sweeps that decrement mass. This result is accounted for by the asymmetry in ion energy absorption profiles as a function of AC frequency and the shift in ion secular frequency at higher amplitudes in the trap due to higher order fields. We also found that use of higher AC amplitudes in forward frequency sweeps biases ions toward ejection at points of higher order parametric resonance, despite using only dipolar excitation. Higher AC amplitudes also increase peak width and decrease sensitivity in both forward and reverse frequency sweeps. Higher sensitivity and resolution were obtained at higher trap pressures in the secular frequency scan, in contrast to conventional resonance ejection scans, which showed the opposite trend in resolution on the Mini 12. Mass range is shown to be naturally extended in secular frequency scanning when ejecting ions by sweeping the AC waveform through low frequencies, a method which is similar, but arguably superior, to the more usual method of mass range extension using low q resonance ejection.

  18. Characterization of protonated phospholipids as fragile ions in quadrupole ion trap mass spectrometry

    PubMed Central

    Garrett, Timothy J.; Merves, Matthew; Yost, Richard A.

    2011-01-01

    Some ions exhibit “ion fragility” in quadrupole ion trap mass spectrometry (QIT-MS) during mass analysis with resonance ejection. In many cases, different ions generated from the same compound exhibit different degrees of ion fragility, with some ions (e.g., the [M+H]+ ion) stable and other ions (e.g., the [M+Na]+ ion) fragile. The ion fragility for quadrupole ion trap (QIT) mass spectrometry (MS) for protonated and sodiated ions of three phospholipids, 1,2-dipalmitoyl-sn-glycero-3-phosphocholine, PC (16:0/16:0), 1,2-dipalmitoyl-sn-glycero-3-phophoethanolamine, PE (16:0/16:0), and N-palmitoyl-D-erythro-sphingosylphosphorylcholine, SM (d18:1/16:0), was determined using three previously developed experiments: 1) the peak width using a slow scan speed, 2) the width of the isolation window for efficient isolation, and 3) the energy required for collision-induced dissociation. In addition, ion fragility studies were designed and performed to explore a correlation between ion fragility in QIT mass analysis and ion fragility during transport between the ion source and the ion trap. These experiments were: 1) evaluating the amount of thermal-induced dissociation as a function of heated capillary temperature, and 2) determining the extent of fragmentation occurring with increasing tube lens voltage. All phospholipid species studied exhibited greater ion fragility as protonated species in ion trap mass analysis than as sodiated species. In addition, the protonated species of both SM (d18:0/16:0) and PC (16:0/16:0) exhibited greater tendencies to fragment at higher heated capillary temperatures and high tube lens voltages, whereas the PE (16:0/16:0) ions did not appear to exhibit fragility during ion transport. PMID:22247650

  19. Experimental Characterization of Secular Frequency Scanning in Ion Trap Mass Spectrometers.

    PubMed

    Snyder, Dalton T; Pulliam, Christopher J; Wiley, Joshua S; Duncan, Jason; Cooks, R Graham

    2016-07-01

    Secular frequency scanning is implemented and characterized using both a benchtop linear ion trap and a miniature rectilinear ion trap mass spectrometer. Separation of tetraalkylammonium ions and those from a mass calibration mixture and from a pesticide mixture is demonstrated with peak widths approaching unit resolution for optimized conditions using the benchtop ion trap. The effects on the spectra of ion trap operating parameters, including waveform amplitude, scan direction, scan rate, and pressure are explored, and peaks at black holes corresponding to nonlinear (higher-order field) resonance points are investigated. Reverse frequency sweeps (increasing mass) on the Mini 12 are shown to result in significantly higher ion ejection efficiency and superior resolution than forward frequency sweeps that decrement mass. This result is accounted for by the asymmetry in ion energy absorption profiles as a function of AC frequency and the shift in ion secular frequency at higher amplitudes in the trap due to higher order fields. We also found that use of higher AC amplitudes in forward frequency sweeps biases ions toward ejection at points of higher order parametric resonance, despite using only dipolar excitation. Higher AC amplitudes also increase peak width and decrease sensitivity in both forward and reverse frequency sweeps. Higher sensitivity and resolution were obtained at higher trap pressures in the secular frequency scan, in contrast to conventional resonance ejection scans, which showed the opposite trend in resolution on the Mini 12. Mass range is shown to be naturally extended in secular frequency scanning when ejecting ions by sweeping the AC waveform through low frequencies, a method which is similar, but arguably superior, to the more usual method of mass range extension using low q resonance ejection. Graphical Abstract ᅟ. PMID:27032650

  20. Extending the Dynamic Range of the Ion Trap by Differential Mobility Filtration

    NASA Astrophysics Data System (ADS)

    Hall, Adam B.; Coy, Stephen L.; Kafle, Amol; Glick, James; Nazarov, Erkinjon; Vouros, Paul

    2013-09-01

    A miniature, planar, differential ion mobility spectrometer (DMS) was interfaced to an LCQ classic ion trap to conduct selective ion filtration prior to mass analysis in order to extend the dynamic range of the trap. Space charge effects are known to limit the functional ion storage capacity of ion trap mass analyzers and this, in turn, can affect the quality of the mass spectral data generated. This problem is further exacerbated in the analysis of mixtures where the indiscriminate introduction of matrix ions results in premature trap saturation with non-targeted species, thereby reducing the number of parent ions that may be used to conduct MS/MS experiments for quantitation or other diagnostic studies. We show that conducting differential mobility-based separations prior to mass analysis allows the isolation of targeted analytes from electrosprayed mixtures preventing the indiscriminate introduction of matrix ions and premature trap saturation with analytically unrelated species. Coupling these two analytical techniques is shown to enhance the detection of a targeted drug metabolite from a biological matrix. In its capacity as a selective ion filter, the DMS can improve the analytical performance of analyzers such as quadrupole (3D or linear) and ion cyclotron resonance (FT-ICR) ion traps that depend on ion accumulation.

  1. Surface ion trap structures with excellent optical access for quantum information processing

    NASA Astrophysics Data System (ADS)

    Maunz, P.; Blain, M.; Benito, F.; Chou, C.; Clark, C.; Descour, M.; Ellis, R.; Haltli, R.; Heller, E.; Kemme, S.; Sterk, J.; Tabakov, B.; Tigges, C.; Stick, D.

    2013-05-01

    Microfabricated surface electrode ion traps are necessary for the advancement of trapped ion quantum information processing as it offers a scalable way for realizing complex trap structures capable of storing and controlling many ions. The most promising way of performing two-qubit quantum gates in a chain of trapped ions is to focus laser beams on individual ions of the chain to drive gates. However, in surface ion traps the close proximity of the ions to the surface and the size of the chips usually cannot accommodate the tightly focused laser beams necessary to address individual ions parallel to the chip surface. Here we present a surface electrode ion trap monolithically fabricated in standard silicon technology that implements a linear quadrupole trap on a bowtie shaped chip with a narrow section that is only 1.2 mm wide. Laser beams parallel to the surface can be focused down to a waist of 4 μm with enough separation from the trap chip to prevent light scattering. The trap structure incorporates two Y-junctions for reordering ions and is optimized for quantum information processing. This work was supported by the Intelligence Advanced Research Projects Activity (IARPA). Sandia National Laboratories is a multi-program laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the US Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

  2. Geometry optimization for the cylindrical ion trap: field calculations, simulations and experiments

    NASA Astrophysics Data System (ADS)

    Wu, Guangxiang; Cooks, R. Graham; Ouyang, Zheng

    2005-03-01

    Optimization of ion trap geometries for best analytical performance was studied in the specific case of the cylindrical ion trap (CIT). An optimization procedure was developed based on field calculations and simulations of ion motion. The electric field inside the CIT was calculated by using the Poisson/Superfish software package and geometrical effects, specifically the half thickness of the ring electrode (zb), the spacing (ds) between the ring electrode and the end-cap electrode, and the end-cap hole radius (rH), were systematically investigated. Appropriate compensation for higher-order field components, namely octapolar and dodecapolar fields, was achieved by refining the CIT geometry and improved mass resolution in scans using boundary and resonance ejection. Resolution for different CIT geometries was measured in both simulations and experiments and was evaluated from the separation between the major isotope peaks of 1,3-dichlorobenzene at m/z 146 and 148. Optimization of the CIT electric field via simple geometry changes involved exploration of several geometries and simulations using the ion trap simulation program (ITSIM) were used to confirm the results for each geometry and to predict experimental performance. Experiments are reported that confirm the enhanced performance achieved using the CITs optimized using the procedure developed in this study.

  3. Extending the Dynamic Range of the Ion Trap by Differential Mobility Filtration

    PubMed Central

    Hall, Adam B.; Coy, Stephen L.; Kafle, Amol; Glick, James; Nazarov, Erkinjon

    2013-01-01

    A miniature, planar, differential ion mobility spectrometer (DMS) was interfaced to an LCQ classic ion trap to conduct selective ion filtration prior to mass analysis in order to extend the dynamic range of the trap. Space charge effects are known to limit the functional ion storage capacity of ion trap mass analyzers and this, in turn, can affect the quality of the mass spectral data generated. This problem is further exacerbated in the analysis of mixtures where the indiscriminate introduction of matrix ions results in premature trap saturation with non-targeted species, thereby reducing the number of parent ions that may be used to conduct MS/MS experiments for quantitation or other diagnostic studies. We show that conducting differential mobility-based separations prior to mass analysis allows the isolation of targeted analytes from electrosprayed mixtures preventing the indiscriminate introduction of matrix ions and premature trap saturation with analytically unrelated species. Coupling these two analytical techniques is shown to enhance the detection of a targeted drug metabolite from a biological matrix. In its capacity as a selective ion filter, the DMS can improve the analytical performance of analyzers such as quadrupole (3-D or linear) and ion cyclotron resonance (FT-ICR) ion traps that depend on ion accumulation. PMID:23797861

  4. Development of a Kingdon ion trap system for trapping externally injected highly charged ions.

    PubMed

    Numadate, Naoki; Okada, Kunihiro; Nakamura, Nobuyuki; Tanuma, Hajime

    2014-10-01

    We have developed a Kingdon ion trap system for the purpose of the laboratory observation of the x-ray forbidden transitions of highly charged ions (HCIs). Externally injected Ar(q+) (q = 5-7) with kinetic energies of 6q keV were successfully trapped in the ion trap. The energy distribution of trapped ions is discussed in detail on the basis of numerical simulations. The combination of the Kingdon ion trap and the time-of-flight mass spectrometer enabled us to measure precise trapping lifetimes of HCIs. As a performance test of the instrument, we measured trapping lifetimes of Ar(q+) (q = 5-7) under a constant number density of H2 and determined the charge-transfer cross sections of Ar(q+)(q = 5, 6)-H2 collision systems at binary collision energies of a few eV. It was confirmed that the present cross section data are consistent with previous data and the values estimated by some scaling formula. PMID:25362383

  5. Development of a Kingdon ion trap system for trapping externally injected highly charged ions

    SciTech Connect

    Numadate, Naoki; Okada, Kunihiro; Nakamura, Nobuyuki; Tanuma, Hajime

    2014-10-01

    We have developed a Kingdon ion trap system for the purpose of the laboratory observation of the x-ray forbidden transitions of highly charged ions (HCIs). Externally injected Ar{sup q+} (q = 5–7) with kinetic energies of 6q keV were successfully trapped in the ion trap. The energy distribution of trapped ions is discussed in detail on the basis of numerical simulations. The combination of the Kingdon ion trap and the time-of-flight mass spectrometer enabled us to measure precise trapping lifetimes of HCIs. As a performance test of the instrument, we measured trapping lifetimes of Ar{sup q+} (q = 5–7) under a constant number density of H₂ and determined the charge-transfer cross sections of Ar{sup q+}(q = 5, 6)-H₂ collision systems at binary collision energies of a few eV. It was confirmed that the present cross section data are consistent with previous data and the values estimated by some scaling formula.

  6. Microfabrication of Surface Ion Trap Chip and State Manipulation of Single 171Yb+ Qubit

    NASA Astrophysics Data System (ADS)

    Hong, Seokjun; Lee, Minjae; Cheon, Hongjin; Ahn, Jun Sik; Kim, Taehyun; Cho, Dong-Il ``Dan''; ASRI/ISRC; Department of Electrical; Computer Engineering, Seoul National University Team; Quantum Tech. Lab., SK Telecom Team

    2015-05-01

    Ion traps are one of the promising physical implementations of quantum information processing. This paper presents new ion trap chips using a copper sacrificial layer. Boundary element method (BEM) simulation results show that the fabricated ion trap chip has a trap depth of 0.063 eV at 81 um above the top electrodes and radial secular frequencies of 1.52 and 1.6 MHz. Up to six 174Yb+ ions and three 171Yb+ ions have been successfully trapped. This paper also demonstrates the state manipulation of single 171Yb+ qubit through Rabi oscillation induced by microwave with frequency of 12.628 GHz. Using the new copper sacrificial method, accurate overhang dimensions that can effectively shield stray electric fields from dielectric layers, which in turn can reduce the micromotion of trapped ions, can be achieved. Acknowledgement: This work was partially supported by ICT R&D program of MSIP/IITP. [10043464, Development of quantum repeater technology for the application to communication systems].

  7. Characterization of odor-active compounds of various Chrysanthemum essential oils by gas chromatography-olfactometry, gas chromatography-mass spectrometry and their correlation with sensory attributes.

    PubMed

    Xiao, Zuobing; Fan, Binbin; Niu, Yunwei; Wu, Minling; Liu, Junhua; Ma, Shengtao

    2016-01-15

    Volatiles of five kinds of Chrysanthemum essential oils with different manufactures were characterized by descriptive sensory analysis, gas chromatography-olfactometry (GC-O), gas chromatography-mass spectrometry (GC-MS) and statistics analysis. Six sensory attributes (floral, woody, grassy, fruity, sour and minty) were selected to assess Chrysanthemum essential oils. A total of 38 volatile compounds were detected and quantified using standard substances by GC-O and GC-MS. Terpenes constituted the largest chemical group among the volatiles of the essential oils. Then partial least squares regression (PLSR) was used to elucidate the relationship between sensory attributes and aroma compounds. The result showed that α-pinene, β-thujene, α-terpinolen, β-cubebene, caryophyllene, (Z)β-farnesene, (-)-spathulenol, linalool, camphor, camphene, 4-terpineol, Z-citral and 4-isopropyltoluene were typical aroma compounds covaried with characteristic aroma of Chrysanthemum essential oils. PMID:26735711

  8. Determination of parts-per-billion concentrations of dioxane in water and soil by purge and trap gas chromatography/mass spectrometry or charcoal tube enrichment gas chromatography

    SciTech Connect

    Epstein, P.S.; Mauer, T.; Wagner, M.; Chase, S.; Giles, B.

    1987-08-01

    Two methods for the determination of 1,4-dioxane in water have been studied. The first method is a heated purge and trap gas chromatography/mass spectrometry system following salting out with sodium sulfate. The second method is an adsorption on coconut-shell charcoal and solvent desorption with carbon disulfide/methanol followed by analysis of the desorbate by gas chromatography with flame ionization detection. The first method is also successful for the determination of 1,4-dioxane in solids and sediments. The second method is shown to be successful for 2-butanone, 4-methyl-2-pentanone, and butoxyethanol in water. The two methods are compared by analyzing 15 samples by both methods and achieving similar results.

  9. Qualitative and quantitative analysis of vetiver essential oils by comprehensive two-dimensional gas chromatography and comprehensive two-dimensional gas chromatography/mass spectrometry.

    PubMed

    Filippi, Jean-Jacques; Belhassen, Emilie; Baldovini, Nicolas; Brevard, Hugues; Meierhenrich, Uwe J

    2013-05-01

    Vetiver essential oils (VEO) are important raw ingredients used in perfume industry, entering the formula of numerous modern fragrances. Vetiver oils are considered to be among the most complex essential oils, resulting most of the time in highly coeluted chromatograms whatever the analytical technique. In this context, conventional gas chromatography has failed to provide a routine tool for the accurate qualitative and quantitative analysis of their constituents. Applying comprehensive two-dimensional gas chromatography techniques (GC×GC-FID/MS) afforded the mean to separate efficiently vetiver oil constituents in order to identify them in a more reliable way. Moreover, this is the first time that a complete true quantitation of each constituent is carried out on such complex oils by means of internal calibration. Finally, we have studied the influence of the injection mode on the determined chemical composition, and showed that several alcohols underwent dehydration under defined chromatographic conditions (splitless mode) usually recommended for quantitation purposes. PMID:23522261

  10. [Analysis of oxygenates from fischer-Tropsch synthesis oil using column liquid chromatography and gas chromatography-mass spectrography].

    PubMed

    Fan, Gaixian; Xu, Yuanyuan; Li, Ying; Li, Ying; Xiang, Hongwei; Li, Yongwang

    2007-11-01

    A liquid chromatographic column filled with silica gel of 100 - 200 mesh was used to separate cold trap oil from Fischer-Tropsch synthesis with dimethylsulfoxide (DMSO) as eluent. With this pretreatment method, the cold trap oil was separated into two major classes, namely, hydrocarbons and oxygenates. Minor components were also enriched and determined, and small peaks adjacent to big peaks and tailings were also well solved. The oxygenates were then analyzed with gas chromatography-mass spectrometry (GC-MS), and 139 components were identified. PMID:18257312

  11. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.

    1989-01-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

  12. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres.

    PubMed

    Valentin, J R

    1989-03-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

  13. The detection of nicotine in a Late Mayan period flask by gas chromatography and liquid chromatography mass spectrometry methods.

    PubMed

    Zagorevski, Dmitri V; Loughmiller-Newman, Jennifer A

    2012-02-29

    Several ancient Mayan vessels from the Kislak Collection of the US Library of Congress were examined for the presence of alkaloids. One of them, a codex-style flask, bears a text that appears to read yo-'OTOT-ti 'u-MAY, spelling y-otoot 'u-may 'the home of its/his/her tobacco'. Samples extracted from this Late Classic period (600 to 900 AD) container were analyzed by gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS) methods. Nicotine was identified as the major component of the extracts. LC/MS analyses also yielded signals due to nicotine mono-oxides. The identities of the compounds were determined by comparison of the chromatographic and/or mass spectral characteristics with those from standards and literature data. High-resolution high mass accuracy tandem mass spectrometry (MS/MS) spectra of protonated nicotine and nicotine mono-oxides were measured to verify and to correct previous product ion assignments. These analyses provided positive evidence for nicotine from a Mayan vessel, indicating it as a likely holder of tobacco leafs. The result of this investigation is the first physical evidence of tobacco from a Mayan container, and only the second example where the vessel content recorded in a Mayan hieroglyphic text has been confirmed directly by chromatography/mass spectrometry trace analysis. PMID:22279016

  14. Identification of epoxide functionalities in protonated monofunctional analytes by using ion/molecule reactions and collision-activated dissociation in different ion trap tandem mass spectrometers.

    PubMed

    Eismin, Ryan J; Fu, Mingkun; Yem, Sonoeun; Widjaja, Fanny; Kenttämaa, Hilkka I

    2012-01-01

    A mass spectrometric method has been delineated for the identification of the epoxide functionalities in unknown monofunctional analytes. This method utilizes gas-phase ion/molecule reactions of protonated analytes with neutral trimethyl borate (TMB) followed by collision-activated dissociation (CAD) in an ion trapping mass spectrometer (tested for a Fourier-transform ion cyclotron resonance and a linear quadrupole ion trap). The ion/molecule reaction involves proton transfer from the protonated analyte to TMB, followed by addition of the analyte to TMB and elimination of methanol. Based on literature, this reaction allows the general identification of oxygen-containing analytes. Vinyl and phenyl epoxides can be differentiated from other oxygen-containing analytes, including other epoxides, based on the loss of a second methanol molecule upon CAD of the addition/methanol elimination product. The only other analytes found to undergo this elimination are some amides but they also lose O = B-R (R = group bound to carbonyl), which allows their identification. On the other hand, other epoxides can be differentiated from vinyl and phenyl epoxides and from other monofunctional analytes based on the loss of (CH(3)O)(2)BOH or formation of protonated (CH(3)O)(2)BOH upon CAD of the addition/methanol elimination product. For propylene oxide and 2,3-dimethyloxirane, the (CH(3)O)(2)BOH fragment is more basic than the hydrocarbon fragment, and the diagnostic ion (CH(3)O)(2)BOH (2) (+) is formed. These reactions involve opening of the epoxide ring. The only other analytes found to undergo (CH(3)O)(2)BOH elimination are carboxylic acids, but they can be differentiated from the rest based on several published ion/molecule reaction methods. Similar results were obtained in the Fourier-transform ion cyclotron resonance and linear quadrupole ion trap mass spectrometer. PMID:22002227

  15. Identification of Epoxide Functionalities in Protonated Monofunctional Analytes by Using Ion/Molecule Reactions and Collision-Activated Dissociation in Different Ion Trap Tandem Mass Spectrometers

    NASA Astrophysics Data System (ADS)

    Eismin, Ryan J.; Fu, Mingkun; Yem, Sonoeun; Widjaja, Fanny; Kenttämaa, Hilkka I.

    2012-01-01

    A mass spectrometric method has been delineated for the identification of the epoxide functionalities in unknown monofunctional analytes. This method utilizes gas-phase ion/molecule reactions of protonated analytes with neutral trimethyl borate (TMB) followed by collision-activated dissociation (CAD) in an ion trapping mass spectrometer (tested for a Fourier-transform ion cyclotron resonance and a linear quadrupole ion trap). The ion/molecule reaction involves proton transfer from the protonated analyte to TMB, followed by addition of the analyte to TMB and elimination of methanol. Based on literature, this reaction allows the general identification of oxygen-containing analytes. Vinyl and phenyl epoxides can be differentiated from other oxygen-containing analytes, including other epoxides, based on the loss of a second methanol molecule upon CAD of the addition/methanol elimination product. The only other analytes found to undergo this elimination are some amides but they also lose O = B-R (R = group bound to carbonyl), which allows their identification. On the other hand, other epoxides can be differentiated from vinyl and phenyl epoxides and from other monofunctional analytes based on the loss of (CH3O)2BOH or formation of protonated (CH3O)2BOH upon CAD of the addition/methanol elimination product. For propylene oxide and 2,3-dimethyloxirane, the (CH3O)2BOH fragment is more basic than the hydrocarbon fragment, and the diagnostic ion (CH3O)2BOH{2/+} is formed. These reactions involve opening of the epoxide ring. The only other analytes found to undergo (CH3O)2BOH elimination are carboxylic acids, but they can be differentiated from the rest based on several published ion/molecule reaction methods. Similar results were obtained in the Fourier-transform ion cyclotron resonance and linear quadrupole ion trap mass spectrometer.

  16. Evaluation of gas-liquid chromatography for the rapid diagnosis of Clostridium difficile associated disease.

    PubMed Central

    Gianfrilli, P; Pantosti, A; Luzzi, I

    1985-01-01

    Direct gas-liquid chromatography of faecal specimens with isocaproic acid as a marker was used for the rapid diagnosis of Clostridium difficile associated diarrhoeal diseases. Ninety stools were examined and results were compared with conventional culture on selective medium and cytotoxin assay in tissue culture. Using a combined analysis of isocaproic acid and butyric acid peak heights we defined three categories: positive, negative, and indeterminate. When the indeterminate group was excluded, the positive and negative predictive values of gas-liquid chromatography analysis were 86.9% and 85% respectively compared with culture and 71.4% and 95% respectively compared with cytotoxin assay. PMID:4008667

  17. Detection of Chemical/Biological Agents and Stimulants using Quadrupole Ion Trap Mass Spectrometry

    SciTech Connect

    Harmon, S.H.; Hart, K.J.; Vass, A.A.; Wise, M.B.; Wolf, D.A.

    1999-06-14

    expanded with additional bacteria and fungi. These spectra were acquired on a Finnigan Magnum ion trap using helium buffer gas. A new database of Cl spectra of microorganisms is planned using the CBMS Block II instrument and air as the buffer gas. Using the current database, the fatty acid composition of the organisms was compared using the percentage of the ion current attributable to fatty acids. The data presented suggest promising rules for discrimination of these organisms. Strain, growth media and vegetative state do contribute to some of the distributions observed in the data. However, the data distributions observed in the current study only reflect our experience to date and do not fully represent the variability that might be expected in practice: Acquisition of MS/ MS spectra has begun (using He and air buffer gas) of the protonated molecular ion of a variety of fatty acids and for a number of ions nominally assigned as fatty acids from microorganisms. These spectra will be used to help verify fatty acid .

  18. PRECISION AND ACCURACY IN THE DETERMINATION OF ORGANICS IN WATER BY FUSED SILICA CAPILLARY COLUMN GAS CHROMOTOGRAPHY/MASS SPECTROMETRY AND PACKED COLUMN GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    Two general methods for the identification and measurement of organic compounds in water are compared. One method employs packed column chromatography and the other fused silica capillary column chromatography. The two gas chromatography/mass spectrometry (GC/MS) methods use diff...

  19. Adsorption of ions onto nanosolids dispersed in liquid crystals: Towards understanding the ion trapping effect in nanocolloids

    NASA Astrophysics Data System (ADS)

    Garbovskiy, Yuriy

    2016-05-01

    The ion capturing effect in liquid crystal nanocolloids was quantified by means of the ion trapping coefficient. The dependence of the ion trapping coefficient on the concentration of nano-dopants and their ionic purity was calculated for a variety of nanosolids dispersed in liquid crystals: carbon nanotubes, graphene nano-flakes, diamond nanoparticles, anatase nanoparticles, and ferroelectric nanoparticles. The proposed method perfectly fits existing experimental data and can be useful in the design of highly efficient ion capturing nanomaterials.

  20. The on-line charge breeding program at TRIUMF's Ion Trap For Atomic and Nuclear Science for precision mass measurements

    SciTech Connect

    Simon, M. C.; Eberhardt, B.; Jang, F.; Luichtl, M.; Robertson, D.; Chaudhuri, A.; Delheij, P.; Grossheim, A.; Kwiatkowski, A. A.; Mane, E.; Pearson, M. R.; Schultz, B. E.; Bale, J. C.; Chowdhury, U.; Ettenauer, S.; Gallant, A. T.; Dilling, J.; Lennarz, A.; Ma, T.; Andreoiu, C.; and others

    2012-02-15

    TRIUMF's Ion Trap for Atomic and Nuclear science (TITAN) constitutes the only high precision mass measurement setup coupled to a rare isotope facility capable of increasing the charge state of short-lived nuclides prior to the actual mass determination in a Penning trap. Recent developments around TITAN's charge breeder, the electron beam ion trap, form the basis for several successful experiments on radioactive isotopes with half-lives as low as 65 ms and in charge states as high as 22+.