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Sample records for chromatographic-mass spectrometric method

  1. Liquid chromatographic-mass spectrometric analysis of glucuronide-conjugated anabolic steroid metabolites: method validation and interlaboratory comparison

    NARCIS (Netherlands)

    Hintikka, L.; Kuuranne, T.; Leinonen, A.; Thevis, M.; Schanzer, W.; Halket, J.; Cowan, D.; Grosse, J.; Hemmersbach, P.; Nielen, M.W.F.; Kostiainen, R.

    2008-01-01

    Liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) method for simultaneous and direct detection of 12 glucuronide-conjugated anabolic androgenic steroid (AAS) metabolites in human urine is described. The compounds selected were the main metabolites detected in huma

  2. A gas chromatographic/mass spectrometric method for the simultaneous quantitation of 5,5-diphenylhydantoin (phenytoin), its para-hydroxylated metabolite and their stable isotope labelled analogs

    International Nuclear Information System (INIS)

    A stable isotope dilution method for the quantitation by GC-MS of 5,5-diphenylhydantoin, its major metabolite (5-(4-hydroxyphenyl)-5-phenylhydantoin), and, simultaneously, their stable isotope labelled analogs (5,5-diphenyl-2-13C-1,3-15N2-hydantoin and 5-(4-hydroxyphenyl)-5-phenyl-2-13C-1,3-15N2-hydantoin) is discussed and evaluated. 5,5-di-(pentadeuterophenyl)hydantoin and 5-(4-hydroxy-3,5-dideuterophenyl)-5-phenyl-2-13C-1,3-15N2-hydantoin are used as internal standards. The chemical work-up procedure of serum (1.0 ml) and urine (0.5 ml) involves acid hydrolysis, extraction at pH 7.4 and permethylation of drug and metabolite analogs by extractive methylation. The mass spectrometric technique consists of repetitive scanning over the molecular ion region of the permethylated derivatives of the phenytoin and para-hydroxy metabolite analogs as they elute from the gas chromatograph. Molecular ion abundances are measured. Reproducibility, selectivity and linearity of the method are discussed in the light of the planned applications. (Auth.)

  3. QuEChERS Method Followed by Solid Phase Extraction Method for Gas Chromatographic-Mass Spectrometric Determination of Polycyclic Aromatic Hydrocarbons in Fish

    Directory of Open Access Journals (Sweden)

    Mona Khorshid

    2015-01-01

    Full Text Available A gas chromatography equipped with mass spectrometer (GCMS method was developed and validated for determination of 16 polycyclic aromatic hydrocarbons (PAHs in fish using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS method for extraction and solid phase extraction for sample cleanup to remove most of the coextract combined with GCMS for determination of low concentration of selected group of PAHs in homogenized fish samples. PAHs were separated on a GCMS with HP-5ms Ultra Inert GC Column (30 m, 0.25 mm, and 0.25 µm. Mean recovery ranged from 56 to 115%. The extraction efficiency was consistent over the entire range where indeno(1,2,3-cdpyrene and benzo(g,h,iperylene showed recovery (65, 69%, respectively, at 2 µg/kg. No significant dispersion of results was observed for the other remaining PAHs and recovery did not differ substantially, and at the lowest and the highest concentrations mean recovery and RSD% showed that most of PAHs were between 70% and 120% with RSD less than 10%. The measurement uncertainty is expressed as expanded uncertainty and in terms of relative standard deviation (at 95% confidence level is ±12%. This method is suitable for laboratories engaged daily in routine analysis of a large number of samples.

  4. Performance evaluation of a thermal desorption/gas chromatographic/mass spectrometric method for the characterization of waste tank headspace samples

    International Nuclear Information System (INIS)

    A thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) method was validated for the determination of volatile organic compounds collected on carbonaceous triple sorbent traps and applied to characterize samples of headspace gases collected from underground nuclear waste storage tanks at the U.S. Department of Energy's Hanford site, in Richland, WA. Method validation used vapor-phase standards generated from 25 target analytes, including alkanes, alkyl alcohols, alkyl ketones, alkylated aromatics, and alkyl nitriles. The target analytes represent a group of compounds identified in one of the most problematic tanks. TD/GC/MS was carried out with modified injectors. Performance was characterized based on desorption efficiency, reproducibility, stability, and linearity of the calibration, method detection limits, preanalytical holding time, and quality control limits for surrogate standard recoveries. Desorption efficiencies were all greater than 82%, and the majority of the analytes (23 out of 25) had reproducibility values less than 24% near the method detection levels. The method was applied to the analysis of a total of 305 samples collected from the headspaces of 48 underground waste storge tanks. Quality control procedures were implemented to monitor sampling and TD/GC/MS method. 33 refs., 2 figs., 4 tabs

  5. A quantitative structure- property relationship of gas chromatographic/mass spectrometric retention data of 85 volatile organic compounds as air pollutant materials by multivariate methods

    Directory of Open Access Journals (Sweden)

    Sarkhosh Maryam

    2012-05-01

    Full Text Available Abstract A quantitative structure-property relationship (QSPR study is suggested for the prediction of retention times of volatile organic compounds. Various kinds of molecular descriptors were calculated to represent the molecular structure of compounds. Modeling of retention times of these compounds as a function of the theoretically derived descriptors was established by multiple linear regression (MLR and artificial neural network (ANN. The stepwise regression was used for the selection of the variables which gives the best-fitted models. After variable selection ANN, MLR methods were used with leave-one-out cross validation for building the regression models. The prediction results are in very good agreement with the experimental values. MLR as the linear regression method shows good ability in the prediction of the retention times of the prediction set. This provided a new and effective method for predicting the chromatography retention index for the volatile organic compounds.

  6. Automatic recognition of polychlorinated biphenyls in gas-chromatographic/mass spectrometric analysis

    International Nuclear Information System (INIS)

    A computer code for automatic recognition of mass spectra of polychlorinated biphenyls (PCBs) has been developed and used as a specific PCB detector in the gas-chromatographic/mass spectrometric analysis. The recognition is based on numerical features to be extracted from the mass spectrum. The code is in Fortran. The result of a classification are the so-called classification chromatograms for the particular groups of PCBs of equal chlorine number. The practical application has been tested on water- and waste oil samples, with PCBs added. The sensitivity is 0,5-1 ng for separate PCB components and 5-20 ng for technical PCD mixtures. 59 refs., 50 figs., 5 tabs. (qui)

  7. Reversed-phase liquid-chromatographic mass spectrometric N-glycan analysis of biopharmaceuticals

    OpenAIRE

    Higel, Fabian; Demelbauer, Uwe; Seidl, Andreas; Friess, Wolfgang; Sörgel, Fritz

    2013-01-01

    N-Glycosylation is a common post-translational modification of monoclonal antibodies with a potential effect on the efficacy and safety of the drugs; detailed knowledge about this glycosylation is therefore crucial. We have developed a reversed-phase liquid chromatographic–mass spectrometric method, with different fluorescent labels, for analysis of N-glycosylation, and compared the sensitivity and selectivity of the methods. Our work demonstrates that anthranilic acid as fluorescent label in...

  8. Automated solid-phase extraction of herbicides from water for gas chromatographic-mass spectrometric analysis

    Science.gov (United States)

    Meyer, M.T.; Mills, M.S.; Thurman, E.M.

    1993-01-01

    An automated solid-phase extraction (SPE) method was developed for the pre-concentration of chloroacetanilide and triazine herbicides, and two triazine metabolites from 100-ml water samples. Breakthrough experiments for the C18 SPE cartridge show that the two triazine metabolites are not fully retained and that increasing flow-rate decreases their retention. Standard curve r2 values of 0.998-1.000 for each compound were consistently obtained and a quantitation level of 0.05 ??g/l was achieved for each compound tested. More than 10,000 surface and ground water samples have been analyzed by this method.

  9. Gas chromatographic/mass spectrometric and microbiological analyses on irradiated chicken

    International Nuclear Information System (INIS)

    Ionizing radiation is widely used as treatment technique for food preservation. It involves among others reduction of microbial contamination, disinfestations, sprout inhibition and extension of shelf life of food. However, the commercialization of irradiated food requires the availability of reliable methods to identify irradiated foodstuffs. In this paper, we present results on the application to irradiated chicken of this method, based on the detection, in muscle and skin samples, of the peaks of ions 98 Da and 112 Da, in a ratio approximately 4:1, typical of radiation induced 2-dodecylcyclobutanones (2-DCB). Aim of the work was also to study the time stability of the measured parameters in samples irradiated at 3 and 5 kGy, and to verify the efficacy of the treatment from a microbiological point of view. Our results show that, one month after irradiation at 3 kGy, the method is suitable using the skin but not the muscle, while the measured parameters are detectable in both samples irradiated at 5 kGy. The microbial population was substantially reduced even at 3 kGy

  10. Gas chromatographic-mass spectrometric determination of ethyl carbamate in alcoholic beverages.

    Science.gov (United States)

    Lau, B P; Weber, D; Page, B D

    1987-07-31

    A sensitive and specific method based on gas chromatography-mass spectrometry for the quantitative determination of ethyl carbamate in table wines, fortified wines (such as ports and sherries), distilled spirits, brandies and liqueurs has been developed. Three characteristic ions from ethyl carbamate [m/z 89 (molecular ion), 74 and 62] were monitored in the selected-ion monitoring (SIM) mode. The lowest detection limit (based on the response on the m/z 62 ion) was estimated to be 0.5 ng/g (ppb). Additional confirmation techniques, including high-resolution SIM, and methane or isobutane chemical ionization are described. PMID:3654867

  11. GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS OF HIGH PURITY SULFUR HEXAFLUORIDE ENRICHED WITH 32S ISOTOPE

    OpenAIRE

    Krylov, V. A.; Sozin, A. Iu.; Chernova, O. Iu.

    2016-01-01

    The method of gas chromatography-mass spectrometry was used for the first time to investigate the impurity composition of high-purity sulfur hexafluoride enriched with 32S isotope. For the separation of impurities an adsorption capillary column GS-GasPro of 60 m ´ 0.32 mm with a modified silica gel and a column of 25 m × 0.26 mm, df = 0.25 microns with  a poly trimethylsilyl propyne (PTMSP) were used. It was shown that GS-GasPro column allowed separating the impurity substances with low molec...

  12. Pilot study of gas chromatographic-mass spectrometric screening of newborn urine for inborn errors of metabolism after treatment with urease.

    Science.gov (United States)

    Kuhara, T; Shinka, T; Inoue, Y; Ohse, M; Zhen-wei, X; Yoshida, I; Inokuchi, T; Yamaguchi, S; Takayanagi, M; Matsumoto, I

    1999-08-01

    Gas chromatographic-mass spectrometric (GC-MS) techniques for urinary organic acid profiling have been applied to high-risk screening for a wide range of diseases, mainly for inborn errors of metabolism (IEM), rather than to low-risk screening or mass screening. Using a simplified procedure with urease-pretreatment and the GC-MS technique, which allows simultaneous determination of organic acids, amino acids, sugars and sugar acids, we performed a pilot study of the application of this procedure to neonatal urine screening for 22 IEM. Out of 16,246 newborns screened, 11 cases of metabolic disorders were chemically diagnosed: two each of methylmalonic aciduria and glyceroluria, four of cystinuria, and one each of Hartnup disease, citrullinemia and alpha-aminoadipic aciduria/alpha-ketoadipic aciduria. The incidence of IEM was thus one per 1477, which was higher than the one per 3000 obtained in the USA in a study targeting amino acids and acylcarnitines in newborn blood spots by tandem mass spectrometry. Also, 227 cases were found to have transient metabolic abnormalities: 108 cases with neonatal tyrosinuria, 99 cases with neonatal galactosuria, and 20 cases with other transient metabolic disorders. Two hundred and thirty-eight cases out of 16,246 neonates (approximately 1/68) were thus diagnosed using this procedure as having either persistent or transient metabolic abnormalities. PMID:10492000

  13. Solid-phase microextraction /gas-chromatographic /mass-spectrometric analysis of p-dichlorobenzene and naphthalene in honey

    OpenAIRE

    Petros A. Tarantilis

    2008-01-01

    Abstract Protection of honey combs from wax moth Galleria mellonella involves the use of physical, biological or chemical control methods. Chemical control may results of residues in the extracted honey. The presence of residues of p-dichlorobenzene and naphthalene in honey were investigated by means of solid-phase microextraction (SPME) coupled to gas-chromatography and mass-spectrometry (GC/MS). The method was linear between 5 ig/kg and 200 ig/kg of honey for p-dichlorobenzene an...

  14. Extraction estimation and gas chromatographic mass spectrometric analysis of the non polar fraction of the pistia stratiotes

    International Nuclear Information System (INIS)

    The non-polar compounds of the Pistia stratiotes were extracted using n-hexane as solvent. The extraction yields were determined both for the cold and hot extraction procedure as 8.50 +- 0.05% and 12.00 +- 0.05%, respectively. The extract was analyzed and separated into its components using GC equipped with FID and GC mass in separate experiments. The most important compounds identified in n-hexane extract of leaves of P. stratiotes are long chain compound of the nitrogenous nature and oxygenated compounds of mixed functional groups. The antibacterial activity of this fraction was investigated against eight pathogenic bacteria using disc diffusion method. Larger zones of inhibition were observed for Bacillus subtilis, Pseudomonas aeruginosa and Agrobacterium tumefaciens as compared to Klebsiella pneumoniaee and Staphylococcus aureus where the activity was relatively less. No activity was observed against Escherichia coli, Salmonella typhi and Bacillus atrophaeus. (author)

  15. Gas chromatographic-mass spectrometric analysis of di(2-ethylhexyl) phthalate and its metabolites in hepatic microsomal incubations

    International Nuclear Information System (INIS)

    A method is reported for the determination of di(2-ethylhexyl) phthalate (DEHP) and its metabolites in in vitro metabolism studies. Gas chromatography-mass spectrometry (GC-MS) analysis allows separation of 18 by-products of DEHP metabolism. On the basis of retention time and specific mass spectra m/z values, three classes of compounds can be identified: (i) alcohols as hydrolysis product; (ii) acids produced by alcohol oxidation; (iii) compounds retaining phthalic moiety. The chromatogram can also be acquired in SIM mode at m/z 149 resulting in 13 well-separated chromatographic peaks: from retention time and mass spectra it can be inferred that the main peaks correspond to mono(2-ethylhexyl) phthalate (MEHP) and (ω-1)-hydroxyl-MEHP. The kinetics of DEHP metabolism was studied using an S9 Aroclor-induced liver fraction as in vitro model and following incubation assay after 20, 40, 60 and 90 min. The composition of incubation mixtures can be quantitatively evaluated from selected ion monitoring chromatograms at m/z 149: the by-product concentration increases during the incubation time, as a consequence of DEHP degradation. During the incubation test a significant conversion of DEHP into MEHP is observed: a conversion yield of 10, 13, 16 and 20% of the original DEHP is obtained after 20, 40, 60 and 90 min, respectively. The metabolic conversion of DEHP to MEHP explains the endocrine-disrupting activity of the original DEHP; moreover, it has been demonstrated that MEHP and its (ω-1)-oxidation metabolite induce peroxisome proliferation. This result strengthens the suggestion that the study of DEHP metabolic pathway is fundamental to better understanding its toxicological behavior

  16. Gas Chromatographic-Mass Spectrometric Analysis of Volatiles Obtained by Four Different Techniques from Salvia rosifolia Sm. and Evaluation for Biological Activity

    Science.gov (United States)

    Volatile constituents from the aerial parts of Salvia rosifolia Sm. (Lamiaceae), endemic to Turkey, were obtained by four different isolation techniques and then analyzed by gas chromatography (GC/FID) and gas chromatography – mass spectrometry (GC/MS) methods. Also in scope of the present work, the...

  17. Liquid-Phase Microextraction and Gas Chromatographic-Mass Spectrometric Analysis of Antidepressants in Vitreous Humor: Study of Matrix Effect of Human and Bovine Vitreous and Saline Solution.

    Science.gov (United States)

    Dos Santos, Marcelo Filonzi; Yamada, Adrian; Seulin, Saskia Carolina; Leyton, Vilma; Pasqualucci, Carlos Augusto Gonçalves; Muñoz, Daniel Romero; Yonamine, Mauricio

    2016-04-01

    In forensic bioanalytical methods, there is a general agreement that calibrators should be prepared by fortifying analytes in matrix-based blank samples (matrix-based). However, in the case of vitreous humor (VH), the collection of blank samples for the validation and for routine analysis would require the availability of many cadavers. Besides the difficulty of obtaining enough blank VH, this procedure could also represent an ethical issue. Here, a study of matrix effect was performed taking into consideration human and bovine vitreous and saline solution (SS) (NaCl 0.9%). Tricyclic antidepressants [amitriptyline (AMI), nortriptyline (NTR), imipramine (IMI) and desipramine (DES)] were used as model analytes and were extracted from samples by means of liquid-phase microextraction and detected by gas chromatography-mass spectrometry. Samples of human and bovine VH and SS were prepared in six different concentrations of antidepressants (5, 40, 80, 120, 160 and 200 ng/mL) and were analyzed. Relative matrix effect was evaluated by applying a two-tailed homoscedastic Student's t-test, comparing the results obtained with the set of data obtained with human VH and bovine VH and SS. No significant matrix effect was found for AMI and NTR in the three evaluated matrices. However, a great variability was observed for IMI and DES for all matrices. Once compatibilities among the matrices were demonstrated, the method was fully validated for AMI and NTR in SS. The method was applied to six VH samples deriving from real cases whose femoral whole blood (FWB) was analyzed by a previously published method. An average ratio (VH/FWB) of ∼0.1 was found for both compounds. PMID:26755541

  18. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  19. Development of Gas Chromatographic Mass Spectrometry.

    Science.gov (United States)

    Hites, Ronald A

    2016-07-19

    Gas chromatographic mass spectrometry is now widely used for the quantitation and identification of organic compounds in almost any imaginable sample. These applications include the measurement of chlorinated dioxins in soil samples, the identification of illicit drugs in human blood, and the quantitation of accelerants in arson investigations, to name just a few. How did GC/MS get so popular? It turns out that it required parallel developments in mass spectrometry, gas chromatography, and computing and that no one person "invented" the technique. This Perspective traces this history from the 1950s until today. PMID:27384908

  20. Determination of actinides by alpha spectrometric methods

    International Nuclear Information System (INIS)

    attributes of mass activities of radionuclides in oyster mushroom's sporocarps compared to their sub-base. We used two methods to separate the monitored radionuclides in a radiochemical analyse. The first of them was an extraction fluid - fluid with Aliquat-336 to separate Pu and TOPO to separate Am. The second method was a proceeding modified by us and utilizing principles of an extraction chromatography with TRU Resin and DGA Resin sorbents made by Eichrom Company. An effectivity and a suitability of both applied methods were monitored following the attributes of radiochemical extractions used in tracer's radionuclides 242Pu a 243Am in this particular type of environmental samples. The reliability of the modified methodology, in accordance to selected criteria for validation of analytical method, was proved by comparison of both above mentioned methods. material delivered from IAEA, which presented a soil sample with code identification Soil IAEA-375. The obtained values of mass activities of 239+240Pu, 239Pu and 241Am used in reference material, demonstrated a conformity with IAEA values, whereby we fulfilled one of the significant conditions of validate process. At the end of this thesis we applied the modified method of extraction chromatography with UTEVA Resin sorbent to define mass activities of uranium on soil and water samples where we monitored attributes of radiochemical extractions of 232U tracer's radionuclide as the criteria of utilizability. The reliability of our modified method was verified by participation in international interlaboratory comparative proficiency tests and our results were in accordance with results of the reference laboratory. It means also a fulfilment of notable standard of the validate process. The results of all realized experimentations of radionuclides separation whether by extraction fluid - fluid or by extraction chromatography were determined by alpha-spectrometric measurements. (author)

  1. Use of mass spectrometric methods for field screening of VOC's

    International Nuclear Information System (INIS)

    While mass spectrometric (MS) methods of chemical analysis, particularly gas chromatography-mass spectrometry (GC/MS), have been the mainstay of environmental organic analytical techniques in the laboratory through the use of EPA and other standard methods, field implementation is relatively rare. Instrumentation and methods now exist for utilizing MS and GC/MS techniques in the field for analysis of VOC's in gas phase, aqueous, and soil media. Examples of field investigations utilizing HP 5971A and Viking SpectraTrak systems for analysis of VOC's in all three media will be presented. Mass spectral methods were found to offer significant advantages in terms of speed of analysis and reliability of compound identification over field gas chromatography (GC) methods while preserving adequate levels of detection sensitivity. The soil method in particular provides a method for rapid in-field analysis of methanol preserved samples thus minimizing the problem of volatiles loss which typically occurs with routine use of the EPA methods and remote analysis. The high cost of MS instrumentation remains a major obstacle to more widespread use

  2. Analysis of dibutylphosphoric acid (DBP) in degraded solvent by utilizing gas chromatograph-mass spectrometry

    International Nuclear Information System (INIS)

    In JAEA, a washing process of tributylphosphate (TBP) in the Purex reprocessing have been investigated by means of n-butylamine oxalate as a washing reagent, which is decomposable by incineration or electrolysis. The concentration of the dibutylphosphoric acid (DBP) in organic and aqueous phase has been determined by an ion-chromatography. In this analytical method, however; we found out that the quantitative analysis for DBP exhibited poor reproducibility because of low sensitivity for DBP. Here we report a new analytical method for DBP by means of a gas chromatograph-mass spectrometry (GC-MS). From our investigation, silylation of DBP was efficient to improve the sensitivity and the reproducibility of the quantitative analysis for DBP. Moreover, we found out that the silylation was effective for the analysis of monobutylphosphoric (MBP). (author)

  3. Gas chromatographic-mass spectrometric analysis of tar compounds formed during pyrolysis of rice husks

    NARCIS (Netherlands)

    Haanappel, V.A.C.; Stevens, T.W.; Hovestad, A.; Skolnik, V.; Visser, R.

    1991-01-01

    Pyrolysis of agricultural waste to produce fuel gas involves formation of tars as noxious by-products. In this paper the qualitative analysis of tars formed during pyrolysis of rice husks is presented, based on identification by gas chromatography—mass spectrometry and interpolation of retention tim

  4. Gas chromatographic-mass spectrometric analysis of tar compounds formed during pyrolysis of rice husks

    OpenAIRE

    Haanappel, V.A.C.; Stevens, T.W.; Hovestad, A.; Skolnik, V.; Visser, R.

    1991-01-01

    Pyrolysis of agricultural waste to produce fuel gas involves formation of tars as noxious by-products. In this paper the qualitative analysis of tars formed during pyrolysis of rice husks is presented, based on identification by gas chromatography—mass spectrometry and interpolation of retention times on a polyaromatic hydrocarbon index scale. The influence of some reaction parameters on product formation is briefly discussed.

  5. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Energy Technology Data Exchange (ETDEWEB)

    Doyle, Adriana [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil); Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N. [Leopoldo Américo Miguez de Mello Research Center — Petrobras (CENPES), Cidade Universitária, Quadra 7, Ilha do Fundão, Rio de Janeiro 21949-900 (Brazil); Aucélio, Ricardo Q., E-mail: aucelior@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil)

    2013-08-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated.

  6. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    International Nuclear Information System (INIS)

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  7. Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: Application to pharmacokinetic studies

    Directory of Open Access Journals (Sweden)

    Issa M

    2008-01-01

    Full Text Available A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III (method I; oxidation of p-aminophenol after the hydrolysis of paracetamol (method II. Iron (II then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 µg/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 µg/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 µg/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

  8. Evaluation of Tamoxifen and metabolites by LC-MS/MS and HPLC Methods

    OpenAIRE

    Heath, D.D.; Flatt, S.W.; Wu, A.H.B.; Pruitt, M.A.; Rock, C.L.

    2014-01-01

    Epidemiological and laboratory evidence suggests that quantification of serum or plasma levels of tamoxifen and the metabolites of tamoxifen, 4-hydroxy-N-desmethyl-tamoxifen (endoxifen), Z-4-hydroxy-tamoxifen (4HT), N-desmethyl-tamoxifen (ND-tam) is a clinically useful tool in the assessment and monitoring of breast cancer status in patients taking adjuvant tamoxifen. A liquid chromatographic mass spectrometric method (LC-MS/MS) was used to measure the blood levels of tamoxifen and the metabo...

  9. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide powder and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Total Carbon by Combustion and Gravimetry 7-17 Total Boron by Titrimetry 18-28 Isotopic Composition by Mass Spectrometry 29-38 Chloride and Fluoride Separation by Pyrohydrolysis 39-45 Chloride by Constant-Current Coulometry 46-54 Fluoride by Ion-Selective Electrode 55-63 Water by Constant-Voltage Coulometry 64-72 Impurities by Spectrochemical Analysis 73-81 Soluble Boron by Titrimetry 82-95 Soluble Carbon by a Manometric Measurement 96-105 Metallic Impurities by a Direct Reader Spectrometric Method 106-114

  10. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.

  11. Recent developments of nanoparticle-based enrichment methods for mass spectrometric analysis in proteomics

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    In proteome research, rapid and effective separation strategies are essential for successful protein identification due to the broad dynamic range of proteins in biological samples. Some important proteins are often expressed in ultra low abundance, thus making the pre-concentration procedure before mass spectrometric analysis prerequisite. The main purpose of enrichment is to isolate target molecules from complex mixtures to reduce sample complexity and facilitate the subsequent analyzing steps. The introduction of nanoparticles into this field has accelerated the development of enrichment methods. In this review, we mainly focus on recent developments of using different nanomaterials for pre-concentration of low-abundance peptides/ proteins, including those containing post-translational modifications, such as phosphorylation and glycosylation, prior to mass spectrometric analysis.

  12. Analysis of medieval glass by X-ray spectrometric methods

    International Nuclear Information System (INIS)

    Systematic investigation of the 16th century glasses of Ljubljana is motivated by the spread of Italian glass-working technology into central Europe. The glass was probed using the external beam PIXE technique due to its non-destructiveness. Initial test measurements were performed by the methods of PIGE, XRF, electron probe microanalysis, and LA-ICP-MS. The PIXE data were evaluated statistically using the principal component analysis and minimizing the stress function. The manufacturing procedures were indicated by the Rb/Sr content in the glass: the investigated glasses were mainly produced with the ash (not potash) of halophitic plants

  13. Extending the frontiers of mass spectrometric instrumentation and methods

    Energy Technology Data Exchange (ETDEWEB)

    Schieffer, Gregg Martin [Iowa State Univ., Ames, IA (United States)

    2010-01-01

    The focus of this dissertation is two-fold: developing novel analysis methods using mass spectrometry and the implementation and characterization of a novel ion mobility mass spectrometry instrumentation. The novel mass spectrometry combines ion trap for ion/ion reactions coupled to an ion mobility cell. The long term goal of this instrumentation is to use ion/ion reactions to probe the structure of gas phase biomolecule ions. The three ion source - ion trap - ion mobility - qTOF mass spectrometer (IT - IM - TOF MS) instrument is described. The analysis of the degradation products in coal (Chapter 2) and the imaging plant metabolites (Appendix III) fall under the methods development category. These projects use existing commercial instrumentation (JEOL AccuTOF MS and Thermo Finnigan LCQ IT, respectively) for the mass analysis of the degraded coal products and the plant metabolites, respectively. The coal degradation paper discusses the use of the DART ion source for fast and easy sample analysis. The sample preparation consisted of a simple 50 fold dilution of the soluble coal products in water and placing the liquid in front of the heated gas stream. This is the first time the DART ion source has been used for analysis of coal. Steven Raders under the guidance of John Verkade came up with the coal degradation projects. Raders performed the coal degradation reactions, worked up the products, and sent them to me. Gregg Schieffer developed the method and wrote the paper demonstrating the use of the DART ion source for the fast and easy sample analysis. The plant metabolite imaging project extends the use of colloidal graphite as a sample coating for atmospheric pressure LDI. DC Perdian and I closely worked together to make this project work. Perdian focused on building the LDI setup whereas Schieffer focused on the MSn analysis of the metabolites. Both Perdian and I took the data featured in the paper. Perdian was the primary writer of the paper and used it as a

  14. Mass spectrometric methods for the direct elemental and isotopic analysis of solid material

    Science.gov (United States)

    Ganeev, A. A.; Gubal, A. R.; Potapov, S. V.; Agafonova, N. N.; Nemets, V. M.

    2016-04-01

    Methods for the direct analysis of solids have a number of undeniable advantages over the methods that require preliminary dissolution of samples. High sensitivity and selectivity make the direct mass spectrometric techniques the most in-demand. The review concerns spark source mass spectrometry, laser ionization mass spectrometry, laser ablation inductively coupled plasma mass spectrometry, secondary ion mass spectrometry, secondary neutral mass spectrometry and glow discharge mass spectrometry. Basic principles, analytical characteristics and trends in the development of these techniques are discussed. Particular attention is given to applications of the techniques as well as to their competitive advantages and drawbacks. The bibliography includes 123 references.

  15. Spectrometric methods used in the calibration of radiodiagnostic measuring instruments

    International Nuclear Information System (INIS)

    Recently a set of parameters for checking the quality of radiation for use in diagnostic radiology was established at the calibration facility of Nederlands Meetinstituut (NMI). The establishment of the radiation quality required re-evaluation of the correction factors for the primary air-kerma standards. Free-air ionisation chambers require several correction factors to measure air-kerma according to its definition. These correction factors were calculated for the NMi free-air chamber by Monte Carlo simulations for monoenergetic photons in the energy range from 10 keV to 320 keV. The actual correction factors follow from weighting these mono-energetic correction factors with the air-kerma spectrum of the photon beam. This paper describes the determination of the photon spectra of the X-ray qualities used for the calibration of dosimetric instruments used in radiodiagnostics. The detector used for these measurements is a planar HPGe-detector, placed in the direct beam of the X-ray machine. To convert the measured pulse height spectrum to the actual photon spectrum corrections must be made for fluorescent photon escape, single and multiple compton scattering inside the detector, and detector efficiency. From the calculated photon spectra a number of parameters of the X-ray beam can be calculated. The calculated first and second half value layer in aluminum and copper are compared with the measured values of these parameters to validate the method of spectrum reconstruction. Moreover the spectrum measurements offer the possibility to calibrate the X-ray generator in terms of maximum high voltage. The maximum photon energy in the spectrum is used as a standard for calibration of kVp-meters

  16. Spectrometric methods used in the calibration of radiodiagnostic measuring instruments

    Energy Technology Data Exchange (ETDEWEB)

    De Vries, W. [Rijksuniversiteit Utrecht (Netherlands)

    1995-12-01

    Recently a set of parameters for checking the quality of radiation for use in diagnostic radiology was established at the calibration facility of Nederlands Meetinstituut (NMI). The establishment of the radiation quality required re-evaluation of the correction factors for the primary air-kerma standards. Free-air ionisation chambers require several correction factors to measure air-kerma according to its definition. These correction factors were calculated for the NMi free-air chamber by Monte Carlo simulations for monoenergetic photons in the energy range from 10 keV to 320 keV. The actual correction factors follow from weighting these mono-energetic correction factors with the air-kerma spectrum of the photon beam. This paper describes the determination of the photon spectra of the X-ray qualities used for the calibration of dosimetric instruments used in radiodiagnostics. The detector used for these measurements is a planar HPGe-detector, placed in the direct beam of the X-ray machine. To convert the measured pulse height spectrum to the actual photon spectrum corrections must be made for fluorescent photon escape, single and multiple compton scattering inside the detector, and detector efficiency. From the calculated photon spectra a number of parameters of the X-ray beam can be calculated. The calculated first and second half value layer in aluminum and copper are compared with the measured values of these parameters to validate the method of spectrum reconstruction. Moreover the spectrum measurements offer the possibility to calibrate the X-ray generator in terms of maximum high voltage. The maximum photon energy in the spectrum is used as a standard for calibration of kVp-meters.

  17. The method for evaluation of irradiated fuel performance based on Gamma - Spectrometric analysis of fission products

    International Nuclear Information System (INIS)

    One of the main aims of International Atomic Energy Agency (IAEA) activities is safeguards control related to the nuclear weapons nonproliferation treaty. To solve this problem, IAEA performs the control of nuclear reactors operation regimes independent of the operator's data. In cases where direct control is impossible, the control of reactor operation regimes may be carried out indirectly by means of spent-fuel parameter investigation. Such spent-fuel parameters as the contents of nuclides 235U, 239Pu, initial fuel enrichment, decay cooling time, and average neutron flux are able to characterize the reactor operation regime. Evaluation of the aforementioned parameters may be carried out utilizing gamma-spectrometric analysis of fission products. Existing methods of gamma-spectrometric data interpretation require information about irradiation history and cooling time after fuel withdrawal. For a research reactor, this information may be incorrect or falsified by the reactor operator; therefore, application of these methods for control of reactor operation regimes is not quite correct. This paper describes a method for spent-fuel parameter evaluation that is based only on utilization of experimental information on ratios of fission product concentrations without data on irradiation history and cooling time

  18. Pretreatment of oily samples for analysis by flow injection-spectrometric methods.

    Science.gov (United States)

    Burguera, José Luis; Burguera, Marcela

    2011-01-15

    This review presents a critical discussion of selected reports dealing with the pretreatment methods of oily samples and the determination of their organic and inorganic constituents using flow systems and spectrometric methods. Special emphasis is given to the on-line couplings with detection systems based on UV-visible spectrophotometry and spectrofluorimetry, atomic absorption spectrometry either with flame or electrothermal atomization as well as inductively coupled plasma optical emission spectrometry or inductively coupled plasma-mass spectrometry. Simple dilution with organic solvents, digestion with concentrated acids under thermal heating, microwave or ultrasound radiation and emulsification procedures are mostly used. The empirical preparation of certain organized assemblies like micelles, emulsions and specially microemulsions added to the confusion of some of the terms, demand a brief description of their characteristics, the correct formulation and some of their applications to the manipulation and treatment of oily samples. The analytical capabilities of combining flow manifolds with spectrometric methods for the determination of specific parameters in oily samples apparently have not been sufficiently exploited yet. PMID:21147308

  19. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 These test methods cover procedures for subsampling and for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride UF6. Most of these test methods are in routine use to determine conformance to UF6 specifications in the Enrichment and Conversion Facilities. 1.2 The analytical procedures in this document appear in the following order: Note 1—Subcommittee C26.05 will confer with C26.02 concerning the renumbered section in Test Methods C761 to determine how concerns with renumbering these sections, as analytical methods are replaced with stand-alone analytical methods, are best addressed in subsequent publications. Sections Subsampling of Uranium Hexafluoride 7 - 10 Gravimetric Determination of Uranium 11 - 19 Titrimetric Determination of Uranium 20 Preparation of High-Purity U3O 8 21 Isotopic Analysis 22 Isotopic Analysis by Double-Standard Mass-Spectrometer Method 23 - 29 Determination of Hydrocarbons, Chlorocarbons, and Partially Substitut...

  20. Mass spectrometric immunoassay

    Science.gov (United States)

    Nelson, Randall W; Williams, Peter; Krone, Jennifer Reeve

    2007-12-04

    Rapid mass spectrometric immunoassay methods for detecting and/or quantifying antibody and antigen analytes utilizing affinity capture to isolate the analytes and internal reference species (for quantification) followed by mass spectrometric analysis of the isolated analyte/internal reference species. Quantification is obtained by normalizing and calibrating obtained mass spectrum against the mass spectrum obtained for an antibody/antigen of known concentration.

  1. Antioxidant activity and gas chromatographic-mass spectrometric analysis of extracts of the marine algae, caulerpa peltata and padina gymnospora

    Directory of Open Access Journals (Sweden)

    Kavitha Murugan

    2014-01-01

    Full Text Available The results of our previous investigations on extracts of selected marine algae showed that Caulerpa peltata and Padina gymnospora had more promising antiproliferative and antioxidant activities than Gelidiella acerosa and Sargassum wightii. Based on these results, the more active chloroform extract of C. peltata and ethyl acetate extract of P. gymnospora were further analyzed for their constituents by using gas chromatography in tandem with mass spectrometry. The GC-MS analysis (GC % peak area given in parentheses showed that fucosterol (12.45% and L-(+-ascorbic acid 2,6-dihexadecanoate (8.13% were the major compounds present in P. gymnospora ethyl acetate extract. On the other hand, C. peltata chloroform extract had 1-heptacosanol (10.52%, hexacosanol acetate (9.28%, tetradecyl ester of chloroacetic acid (7.22%, Z,Z-6,28-heptatriactontadien-2-one (6.77% and 10,13-dimethyl-methyl ester of tetradecanoic acid (5.34% as major compounds. Also described in the report are the beta-carotene bleaching inhibitory and total reducing activities of the chloroform and ethyl acetate extracts of C. peltata and P. gymnospora, respectively, relative to the other three extracts (aqueous, methanol, chloroform or ethyl acetate of the two algae.

  2. Enhanced recognition of spin trapped radicals in complex mixtures: Deuterated nitronyl adducts provide a gas chromatographic/mass spectrometric marker

    International Nuclear Information System (INIS)

    The use of deuterated analogues of α-phenyl-N-tert-butyl nitrone (PBN) are reported for GC/MS analysis of spin trapping products. PBN-d9 and PBN-d14, deuterated in the tert-butyl group (the latter also deuterated in the phenyl ring), result in a more diagnostic fragment ion, C4D9+ (m/z = 66) which improves the recognition of PBN adducts in mixtures. This feature has helped identify a new 1,3-radical addition product of PBN-d9 formed during azobis(isobutyronitrile) thermolysis (addition of 2-cyano-2-propyloxyl followed by 2-cyano-2-propyl radicals). The 13C-trichloromethyl radical adduct of PBN-d14 produced during 13C-carbon tetrachloride incubation with rat liver microsomes was identified by GC/MS in a complicated biological extract mixture. 25 refs., 3 figs., 1 tab

  3. Liquid chromatographic-mass spectrometric analysis of anthocyanin composition of dark blue bee pollen from Echium plantagineum.

    Science.gov (United States)

    Di Paola-Naranjo, Romina Daniela; Sánchez-Sánchez, José; González-Paramás, Ana María; Rivas-Gonzalo, Julián Carlos

    2004-10-29

    Dark blue bee pollen samples from pollinic type Echium plantegineum were analysed in order to identify and quantify their anthocyanin pigments. Five samples were collected from different apicultural Spanish regions and the anthocyanin composition was determined by HPLC with diode array and MS detection. Eight different pigments were identified, the principal anthocyanin being petunidin-3-O-rutinoside. The other pigments found were delphinidin, cyanidin and petunidin-3-O-glucoside; delphinidin, cyanidin, peonidin and malvidin-3-O-rutinoside and cyanidin-3-(6"-malonylglucoside). The anthocyanin content ranged from 45 to 80 mg/100 g of blue pollen, which could represent a significant source of phytochemicals. Minor variations in the anthocyanin profiles were found, which could be explained by the geographical differences between collection regions. PMID:15553145

  4. A gas chromatographic-mass spectrometric approach to examining stereoselective interaction of human plasma proteins with soman.

    Science.gov (United States)

    Yeung, David T; Smith, J Richard; Sweeney, Richard E; Lenz, David E; Cerasoli, Douglas M

    2008-01-01

    The organophosphorus (OP) nerve agent soman (GD) contains two chiral centers (a carbon and a phosphorus atom), resulting in four stereoisomers (C+P+, C-P+, C+P-, and C-P-); the P- isomers exhibit a mammalian toxicity that is approximately 1000-fold greater than that of the P+ isomers. The capacity to assess the binding or hydrolysis of each of the four stereoisomers is an important tool in the development of enzymes with the potential to protect against GD intoxication. Using a gas chromatography-mass spectrometry-based approach, we have examined the capacity of plasma-derived human serum albumin, plasma-purified human butyrylcholinesterase, goat milk-derived recombinant human butyrylcholinesterase, and recombinant human paraoxonase 1 to interact with each of the four stereoisomers of GD in vitro at pH 7.4 and 25 degrees C. Under these experimental conditions, the butyrylcholinesterase samples were found to bind GD with a relative preference for the more toxic stereoisomers (C-P- > C+P- > C-P+ > C+P+), while human serum albumin and paraoxonase 1 interacted with GD with a relative preference for the less toxic isomers (C-P+/C+P+ > C+P-/C-P-). The results indicate that these human proteins exhibit distinct stereoselective interactions with GD. The approach described presents a means to rapidly assess substrate stereospecificity, supporting future efforts to develop more effective OP bioscavenger proteins. PMID:18269799

  5. Gas chromatographic mass spectrometric analysis of n-hexane fraction of the leaves of sugar beets (beta vulgarus)

    International Nuclear Information System (INIS)

    The n-hexane fraction of the leaves of sugar beet was analyzed qualitatively and quantitatively using GC-MS and GC equipped with FID in separate experiments. The crude was extracted using ethanol and fractionated by n-hexane, ethyl acetate and chloroform in the increasing order of polarity. Only the n-hexane fraction was analyzed using GC-MS and GC equipped with FID. The nature of products was confirmed using total ion chromatograms as well as fragmentation pattern. The concentration of the major compounds was determined using the peak area. The n-hexane fraction was found to contain esters in addition to small quantities of other compounds. (author)

  6. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    OpenAIRE

    Hou, Xiaolin; Roos, Per

    2008-01-01

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for rad...

  7. A simple method for determination of formaldehyde in seafood sample using spectrometric detection

    International Nuclear Information System (INIS)

    Complete text of publication follows. A simple method for determination of formaldehyde using spectrometric detection was developed. The reaction was based on the oxidation of methylene blue with hydrogen peroxide in acidic media. The decreased in absorbance of the reaction mixture was measured at 664 nm. The optimum reaction conditions were 1 x 10-6 M methylene blue, 0.01 M sulfuric acid and 0.02 M hydrogen peroxide. The linearity was 0-20 mg/l with the limit of determination 1.60 μg/g of sample. Extraction of formaldehyde in seafood samples were investigated by ultrasonic method. The percentage recovery in spiking sample was 98% with 30 min ultrasonic extraction. This proposed method was applied to determination of formaldehyde in seafood samples. The researcher gratefully acknowledge the support from Center of Excellence for Innovation in Chemistry (PERCH-CIC), Commission on Higher Education, Ministry of Education.

  8. Characterisation of radioactive contaminated materials by combined radiometric and spectrometric methods

    International Nuclear Information System (INIS)

    In the present paper, a combined analytical methodology is described, for characterization of radioactive contaminated materials. The subject of testing activities was a set of solutions provided by the Cernavoda NPP, which are originating from processes of radiological survey of workplaces in the plant. In the introduction section, a theoretical approach was given to the origin and nature of main radionuclides occurring in the primary cooling system of the nuclear power plant, with the aim to establish selection criteria and performance requirements for the analytical methods to be used in the development of the characterization methodology. A combination of radiometric and spectrometric methods was selected, based on gross beta counting, high resolution gamma-ray spectrometry and liquid scintillation counting. (authors)

  9. Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum (LLE-GCMS)and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoyan; GAO Naiyun; CHEN Beibei; LI Qingsong; ZHANG Qiaoli; GU Guofen

    2007-01-01

    Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction (SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum (GCMS) in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol (2-MIB)and geosmin (GSM) with values below 50%.For LLE,the recoveries were satisfyingly above 50% for 2-MIB and 80% for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.

  10. Standard test methods for chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide (Gd2O3) powder

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Carbon by Direct CombustionThermal Conductivity C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Total Chlorine and Fluorine by Pyrohydrolysis Ion Selective Electrode C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Loss of Weight on Ignition 7-13 Sulfur by CombustionIodometric Titration Impurity Elements by a Spark-Source Mass Spectrographic C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical,Nuclear, and Radiochemical Analysis of Uranium Hexafluoride C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry Gadolinium Content in Gadolinium Oxid...

  11. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  12. Analytical Method Validation of Gamma Spectrometric Procedure for the Determination of γ-Emitters in Environmental Samples

    International Nuclear Information System (INIS)

    It is internationally recognized that validation is necessary in analytical laboratories. The use of validated methods is important for an analytical laboratory to show its qualification and competency. This work describes the methods for validation of gamma spectrometric analytical procedure in the determination of some gamma emitters in environmental samples. The method was tested and validated in terms of repeatability, trueness, reproducibility in accordance with ISO guidelines using IAEA reference materials with different matrixes and compositions

  13. Method of double tracer addition for determining uranium in geological samples by mass spectrometric isotope dilution

    International Nuclear Information System (INIS)

    The present work shows the experimental details on the uranium determination in materials by mass spectrometric isotope dilution technique with double tracer (233U + 235U). The mass discrimination phenomenon effect is studied. The uranium concentration values obtained by mass spectrometric isotope dilution technique with double tracer are compared with other techniques. The influence of the sampling in the accurate determination of uranium in the rock sample is discussed. (author)

  14. On the reliability of methods for the speciation of mercury based on chromatographic separation coupled to atomic spectrometric detection

    OpenAIRE

    Qvarnström, Johanna

    2003-01-01

    This thesis deals with the reliability of methods for the speciation of mercury in environmental and biological samples. Problems with speciation methods that couple chromatography to atomic spectrometric detection and how to overcome the problems are discussed. Analytical techniques primarily studied and evaluated are high performance liquid chromatography-cold vapour-atomic absorption spectrometry (HPLC-CV-AAS), HPLC-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), capillary elec...

  15. A spectrometrical method to measure the deuterium content in 2H-enriched water

    International Nuclear Information System (INIS)

    A test method and spectrometer has been developed for emission-spectrometrical measurement of the deuterium content in water enriched with deuterium. The water sample is melted into a previously evacuated glas tube and a gas discharge is excited in vapour over the cooled sample to adjust to a low vapour pressure with high frequency. The intensities of the H(α) and D(α) lines appearing in the spectrum determine the D-content. Both lines were resolved by a Fabry-Perot interferometer and geometrically separated fed to two photodetectors. The remaining spectrum is filtered off. Following electronic calculation of the signals, the measured value is indicated which has to be corrected by a standard curve. The relative measuring accuracy is about +-1% for enrichments of over 1% D and less than +-5% in the region of 0.3-1% D. The detection limit is about 0.03% D (sample amount: 50 μl, average of 5 samples). (orig./HP)

  16. Determination of U and Th content in the zirconium purification process using alpha spectrometric method

    International Nuclear Information System (INIS)

    It has been performed determination of U and Th and decay daughter in the zirconium purification process using alpha spectrometric method. U and Th analysis applications as well as decay daughter of zirconium purification process done, from Na2ZrO3 dissolved stage, Na2ZrO3 dissolved with 4 M HCl, dissolving Chloride Zircon Oxide (ZOC) with 6M H2SO4 at 105°C the heating. The purpose of this study is to determine the concentration of U and Th and decay daughter of Na2ZrO3 dissolved process, Na2ZrO3 dissolved with 4 M HCl, dissolving Chlorid Zircon oxide (ZOC) with 6M H2SO4 at 105° C the heating. From the experiments it can be concluded that the Na2ZrO3 solution and ZrOCI2, there is no U and Th nuclides, where as in solution Zr5O8(SO4)2 there are U and Th content. (author)

  17. Toward a Micro Gas Chromatograph/Mass Spectrometer (GC/MS) System

    Science.gov (United States)

    Wiberg, D. V.; Eyre, F. B.; Orient, O.; Chutjian, A.; Garkarian, V.

    2001-01-01

    Miniature mass filters (e.g., quadrupoles, ion traps) have been the subject of several miniaturization efforts. A project is currently in progress at JPL to develop a miniaturized Gas Chromatograph/Mass Spectrometer (GC/MS) system, incorporating and/or developing miniature system components including turbomolecular pumps, scroll type roughing pump, quadrupole mass filter, gas chromatograph, precision power supply and other electronic components. The preponderance of the system elements will be fabricated using microelectromechanical systems (MEMS) techniques. The quadrupole mass filter will be fabricated using an X-ray lithography technique producing high precision, 5x5 arrays of quadrupoles with pole lengths of about 3 mm and a total volume of 27 cubic mm. The miniature scroll pump will also be fabricated using X-ray lithography producing arrays of scroll stages about 3 mm in diameter. The target detection range for the mass spectrometer is 1 to 300 atomic mass units (AMU) with are solution of 0.5 AMU. This resolution will allow isotopic characterization for geochronology, atmospheric studies and other science efforts dependant on the understanding of isotope ratios of chemical species. This paper will discuss the design approach, the current state-of-the art regarding the system components and the progress toward development of key elements. The full system is anticipated to be small enough in mass, volume and power consumption to allow in situ chemical analysis on highly miniaturized science craft for geochronology, atmospheric characterization and detection of life experiments applicable to outer planet roadmap missions.

  18. Gas chromatographic mass analysis and further pharmacological actions of Cymbopogon proximus essential oil.

    Science.gov (United States)

    Al-Taweel, A M; Fawzy, G A; Perveen, S; El Tahir, K E H

    2013-09-01

    The present study reports Gas chromatographic mass analysis (GC-MS) as well as important biological activities of Cymbopogon proximus essential oil. The chemical composition of the essential oil of Cymbopogon proximus was investigated by GC-MS. Furthermore, the effects of Cymbopogon proximus essential oil on the cardiac parasympathetic ganglia in rats, the intra-tracheal pressure in guinea-pigs and on carrageenan-induced inflammation in the rats paw, were studied. The GC-MS study led to the identification of 22 components with Piperitone representing (73.81%), Elemol (9.32%), alpha-Eudesmol (5.21%) and alpha-Terpineol (3.01%) of the oils composition. The percentage protective effect of the oil on the vagus-induced bradycardia in rats was 90.1±3.1%, which represents a significant protection. As for the effect of Cymbopogon oil on bronchoconstrictors-induced increase in intra-tracheal pressure in guinea-pigs, the oil antagonized the actions of 5-HT and histamine by 80±3.7 and 93±8.3%, respectively. Pharmacological investigations using Cymbopogon oil revealed its inherent ability to possess a bronchodilator activity mediated via blockade of both histamine and serotonin receptors. It possessed a significant ganglionic blocking action and a limited anti-inflammatory activity that seemed to involve blockade of histamine and serotonin receptors in the rats' paws. PMID:23780497

  19. Study of precious metal-bearing rocks by inductively coupled plasma spectrometric methods

    International Nuclear Information System (INIS)

    Complete text of publication follows. This topic involves the determination of Pt and Pd content of precious metal-bearing rocks (from the Sudbury magmatic complex) by inductively coupled plasma spectrometric methods. Altogether 9 samples were available for the comparison of recoveries by lead fire assay and decomposition by aqua regia. The standard analytical method for the determination of platinum group elements in the Laboratory of GIH is ICP-OES and ICP-MS analysis after aqua regia decomposition. The matrix was very heavy, up to 35% in Cu; 30% in Fe and 3% in Ni. A JY ULTIMA 2C ICP-OES instrument was used for the determination of Pt and Pd content from the aqua regia solution. Although this instrument has a very good spectral resolution (5 pm), the straight analysis is not easy in a complicated, line-rich matrix. The background positions were changing at most of the samples, therefore graphical evaluation was the best for subtracting the proper background values. Several analytical lines were used for the determination of Pt and Pd. The Pt and Pd contents were also analysed by ICP-MS (Perkin-Elmer ELAN DRC II) on different isotopes. The different Pd isotopes supplied different concentrations indicating that spectral overlaps made the strait analysis very difficult and uncertain. There was a possibility within a bilateral scientific cooperation with the South Vietnam Geological Mapping Division of Analysis and Experiment (Ho Chi Minh City) to complete lead fire assay procedures from these samples. After dissolving the silver prill at the end of the procedure the ICP-OES and the ICP-MS analysis were performed again from the relatively matrix-free solutions. The results of the 2 decompositions were compared.

  20. A method to evaluate gamma-spectrometric measurements of NORM samples

    International Nuclear Information System (INIS)

    Although a detailed and well-defined monitoring programme should be carried out in order to evaluate properly occupational doses in industrial activities involving NORM, a first estimation about the dose levels susceptible to be received by the workers can be performed with basis in the knowledge of the radioactivity content of the materials involved or produced in the analysed industrial processes (ores, by-products, scales, sludges,..). The dose estimations performed through the commented approach demand the application of proper and accurate measuring techniques. In this sense, it is well known that gamma-ray spectrometry provides a fast and simple method for the measurement of a good set of natural radionuclides belonging to the Uranium and Thorium series. The multi-elemental and non-destructive character of this technique makes it superior, in many cases, to more traditional and skill based radiochemical procedures. Nevertheless, two main tasks arise when this technique should be applied for the measurement of NORM samples: a) the proper management and interpretation of the complex gamma-ray spectra obtained from the measurements, and b) the accurate determination of the photopeak efficiencies at different energies for each sample. This last task is far from be straightforward in a laboratory devoted to the measurement of NORM samples due to their great variability in the available amounts of material (geometry source-detector) and in their densities (self-absorption). In the present work the method used in our laboratory to evaluate the gamma-spectrometric measurements of NORM samples is detailed. This method is based in the determination for each sample of the photopeak efficiency versus energy curve by applying a Monte Carlo simulation (using the GEANT4 simulation toolkit) and in the application of a procedure for correcting serious spectral interferences present on several gamma-ray peaks of interest. The whole method has been checked via the analysis of

  1. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    International Nuclear Information System (INIS)

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  2. Sublimation as a Method of Matrix Application for Mass Spectrometric Imaging

    OpenAIRE

    Hankin, Joseph A.; Barkley, Robert M.; Murphy, Robert C.

    2007-01-01

    Common organic MALDI matrices, 2,5-dihydroxybenzoic acid, 3,5-dimethoxy-4-hydroxycinnamic acid, and alpha-cyano-4-hydroxy-cinnamic acid were found to undergo sublimation without decomposition under conditions of reduced pressure and elevated temperature. This solid to vapor phase transition was exploited to apply MALDI matrix onto tissue samples over a broad surface in a solvent-free application for mass spectrometric imaging. Sublimation of matrix produced an even layer of small crystals acr...

  3. A Chemical Eight Group Separation Method for Routine Use in Gamma Spectrometric Analysis. II. Detailed analytical schema

    International Nuclear Information System (INIS)

    A detailed ion-exchange procedure for the separation of chemical elements in eight groups suitable for subsequent gamma spectrometric analysis is described. The method has been in use for gamma spectrometry of some inorganic - but mostly organic - samples for one year. The separation time for inorganic samples, is usually about 1.5 hours and for organic samples as least 2 hours. One man can separate and count three samples per day. In comparative measurements of short-lived isotopes in biological material 10-12 elements can be analysed thus making possible 30 - 35 determinations per day for one man

  4. Mass spectrometric methods for studying nutrient mineral and trace element absorption and metabolism in humans using stable isotopes: a review

    International Nuclear Information System (INIS)

    Mass spectrometric methods for determining stable isotopes of nutrient minerals and trace elements in human metabolic studies are described and discussed. The advantages and disadvantages of the techniques of electron ionization, fast atom bombardment, thermal ionization, and inductively coupled plasma and gas chromatography mass spectrometry are evaluated with reference to their accuracy, precision, sensitivity, and convenience, and the demands of human nutrition research. Examples of specific applications are described and the significance of current developments in mass spectrometry are discussed with reference to present and probable future research needs. (Author)

  5. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Plutonium by Controlled-Potential Coulometry Plutonium by Amperometric Titration with Iron(II) Plutonium by Diode Array Spectrophotometry Free Acid by Titration in an Oxalate Solution 8 to 15 Free Acid by Iodate Precipitation-Potentiometric Titration Test Method 16 to 22 Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33 Thorium by Thorin Spectrophotometric Test Method 34 to 42 Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50 Impurities by ICP-AES Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58 Fluoride by Distillation-Spectrophotometric Test Method 59 to 66 Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74 Isotopic Composition by Mass Spectrom...

  6. Chemotrapping-atomic fluorescence spectrometric method as a field method for volatile arsenic in natural gas.

    Science.gov (United States)

    Uroic, M Kalle; Krupp, Eva M; Johnson, Charlie; Feldmann, Jörg

    2009-12-01

    Volatile arsenic compounds in natural gas, existing in the form of trimethylarsine (TMAs), have been determined using gas cryo-trapping gas chromatography coupled to inductively coupled plasma-mass spectrometry (CT-GC-ICP-MS). The results from a number of different gas wells revealed a huge concentration spread ranging from below the detection limit of 0.2 up to 1800 microg/m(3) TMAs (as As) in the gas. Due to the toxicity and corrosive nature of these arsines, they need near real time monitoring via a method that can easily be implemented on site, i.e. during gas exploitation. Here, we introduce a novel method which utilises silver nitrate impregnated silica gel tubes for quantitative chemotrapping of trimethylarsine (TMAs) from a natural gas matrix. Subsequent elution with hot nitric acid followed by online photo-oxidation hydride generation atomic fluorescence spectrometry (HG-AFS) is used for the determination of TMAs gas standards in nitrogen and natural gas samples, respectively. The chemotrapping method was validated using CT-GC-ICP-MS as a reference method. The recovery of arsenic from nitrogen or natural gas matrix ranged from 85 to 113% for a range of 20 to 2000 ng As. Trapping efficiency was >98%, from the methods LOD of 20 ng to 4.8 microg (absolute amount As) with sample sizes of 0.02 and 2 L gas. Method performance was established by comparing the results obtained for eight natural gas samples containing between 1 and 140 microg As/m(3) with those achieved by the reference method (CT-GC-ICP-MS). PMID:20024020

  7. Standard methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal

    International Nuclear Information System (INIS)

    Methods are described for the analysis of matrix materials and various impurities in Pu metal. Controlled-potential coulometry, amperometric titration with Fe2+, or titration with ceric sulfate methods are described for the determination of Pu. A mass spectrometric method is given for determination of the isotopic content of the metal. Determination of C by direct combustion-thermal conductivity is described. Methods for the spectrophotometric determination of U with arsenazo I, Th with thorin, Fe with 1,10-phenanthroline or α,α'-dipyridyl, and Cl-, F-, N, and S following separation by distillation are described. If the Pu metal does not contain significant amounts of other radioactive fission products or high specific-activity γ emitters, 241Am may be determined by γ counting. Determination of γ-emitting fission products, U and Th, is determined by γ spectroscopy. Spectrochemical methods for the determination of rare earths, W, Nb, Ta, and about 40 other trace elements are included

  8. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples.

    Science.gov (United States)

    Hou, Xiaolin; Roos, Per

    2008-02-11

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry, resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer application in the environmental and biological researches, these radionuclides include (3)H, (14)C, (36)Cl, (41)Ca, (59,63)Ni, (89,90)Sr, (99)Tc, (129)I, (135,137)Cs, (210)Pb, (226,228)Ra, (237)Np, (241)Am, and isotopes of thorium, uranium and plutonium. The application of on-line methods (flow injection/sequential injection) for separation of radionuclides and automated determination of radionuclides is also discussed. PMID:18215644

  9. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solutions

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1999-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Determination of Uranium 7 Specific Gravity by Pycnometry 15-20 Free Acid by Oxalate Complexation 21-27 Determination of Thorium 28 Determination of Chromium 29 Determination of Molybdenum 30 Halogens Separation by Steam Distillation 31-35 Fluoride by Specific Ion Electrode 36-42 Halogen Distillate Analysis: Chloride, Bromide, and Iodide by Amperometric Microtitrimetry 43 Determination of Chloride and Bromide 44 Determination of Sulfur by X-Ray Fluorescence 45 Sulfate Sulfur by (Photometric) Turbidimetry 46 Phosphorus by the Molybdenum Blue (Photometric) Method 54-61 Silicon by the Molybdenum Blue (Photometric) Method 62-69 Carbon by Persulfate Oxidation-Acid Titrimetry 70 Conversion to U3O8 71-74 Boron by ...

  10. Mass spectrometric and high-performance liquid chromatographic studies of medroxyprogesterone acetate metabolites in human plasma.

    Science.gov (United States)

    Sturm, G; Häberlein, H; Bauer, T; Plaum, T; Stalker, D J

    1991-01-01

    Medroxyprogesterone acetate (MPA) treatment has been shown to exert several beneficial effects in cancer patients. It has been suggested that such effects are due in part to the metabolites derived from MPA in vivo. The first results are reported on the identification of 2 alpha-hydroxy- and 21-hydroxy-MPA, 20-dihydro-MPA, 17 alpha-acetoxy-2 alpha,3 beta-dihydroxy-6 alpha-methylpregn-1,4-dien-20-one and two X,21-dihydroxy-MPAs, one of them presumably being 6 alpha-hydroxymethyl-21-hydroxy-MPA, in patient's plasma by high-performance liquid chromatographic (HPLC), gas chromatographic-mass spectrometric and NMR methods. Additionally, the presence of other metabolites such as di- and tetrahydro-MPAs and 6,21-dihydroxy-MPA, found in urine and other samples, was demonstrated in plasma. For routine clinical examinations an HPLC method is described for determination of, e.g., the unreduced MPA metabolite group in Sep-Pak-ODS column extracts of patients' plasma. PMID:1827448

  11. Characterization of 241Am and Pu content in soil from peaceful nuclear explosions regions by γ/X-spectrometric method

    International Nuclear Information System (INIS)

    The γ/X-spectrometric methodology and apparatus for analysis of the 241Am content in the soil and plant samples from the peaceful nuclear explosions areas in Yakutiya and the Perm region are briefly presented. The conclusion is made on the possibility of applying the γ/X-spectrometric methodology for the wide-scale measurements in the peaceful nuclear explosions regions

  12. Thermodynamic properties of the UO2-ZrO2 system studied by the isothermal mass spectrometric vaporization method

    International Nuclear Information System (INIS)

    The Knudsen effusion high-temperature mass spectrometric method was used to study the vaporization processes and thermodynamic properties of the UO2-ZrO2 system in the temperature range 2200-2650 K. The work was carried out with the MS 1301 mass spectrometer developed for studies of physico-chemical properties of inorganic substances at high temperatures. Vaporization of the solid solutions containing 0.02-0.45 mol fractions of UO2 was done using tungsten cells. The vaporization processes and the chemical potentials of ZrO2 in the UO2-ZrO2 system and in the Y2O3-ZrO2, Lu2O3-ZrO2 and HfO2-ZrO2 systems, available in the literature, were discussed from the point of view of the acid-base concept. (orig.)

  13. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Plutonium Sample Handling 8 to 10 Plutonium by Controlled-Potential Coulometry Plutonium by Ceric Sulfate Titration Plutonium by Amperometric Titration with Iron(II) Plutonium by Diode Array Spectrophotometry Nitrogen by Distillation Spectrophotometry Using Nessler Reagent 11 to 18 Carbon (Total) by Direct Combustion–Thermal Conductivity 19 to 30 Total Chlorine and Fluorine by Pyrohydrolysis 31 to 38 Sulfur by Distillation Spectrophotometry 39 to 47 Plutonium Isotopic Analysis by Mass Spectrometry Rare Earth Elements by Spectroscopy 48 to 55 Trace Elements by Carrier–Distillation Spectroscopy 56 to 63 Impurities by ICP-AES Impurity Elements by Spark-Source Mass Spectrography 64 to 70 Moisture by the Coulomet...

  14. Differentiation of the four major types (C. Burmannii, C. Verum, C. cassia, And C. Loureiroi) of cinnamons using a flow-injection mass spectrometric (FIMS) fingerprinting method

    Science.gov (United States)

    A simple and efficient flow-injection mass spectrometric (FIMS) method was developed to differentiate cinnamon (Cinnamomum) bark (CB) samples of the four major species (C. burmannii, C. verum, C. aromaticum, and C. loureiroi) of cinnamon. Fifty cinnamon samples collected from China, Vietnam, Indon...

  15. Radioisotope spectrometric method to determine diffusion coefficients in metals and alloys

    International Nuclear Information System (INIS)

    A brief description of the spectrometric installation to study diffusion in metals using #betta#-decay radio-isotopes is presented. Diffusion coefficients of nickel in 70% Co-5% Fe-15% Si-10% B amorphous alloy are determined according to #betta#-radiation absorption in diffusion zone. Plate samples of 10x10 mm size and about 300 μm in thickness are used. Diffusion annealing is conducted during 100 hrs. The calculation of the diffusion coefficients has been carried out by the formula I/I0= esup(μsup(2)Dtau)erfc μ √ Dtau, where I0, I is an initial and a final radiation intensity; μ- an absorption coefficient of 63Ni #betta#-ray in the given material (at calculation μ=1.3x106 m-1 was taken); tau- duration of diffusion annealing; D- diffusion coefficient at the designed temperature. The value of the diffusion coefficient of nickel in 70% Co-5% Fe-15% S-10% B amorphous alloy at the temperature of 200 deg C is turned out to be equal to 4x10-21 m2/s. It should be noted that the self-diffusion coefficient of cobalt in Co-Fe alloy, found by extrapolation from high-temperature region, is equal to 10-35 m2/s, i.e. in 14 orders lower than that of the same basis in amorphous alloy

  16. Standard methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets

    International Nuclear Information System (INIS)

    Various methods are described in detail as to procedure, interferences, and limits of detection or applicability for the determination of Pu and various impurities in PuO2 powders and pellets. Methods for the determination of Pu are controlled-potential coulometry, ceric sulfate titration, and amperometric titration with Fe2+. Spectrophotometric methods are given for N and S, and a direct combustion-thermal conductivity method for the determination of total C is described. A pyrohydrolysis method is described for the determination of μg amounts of Cl- and F-. A mass spectrometric determination of the Pu isotopic content of the oxide is included, and general chemical methods are included for the determination of moisture in both powders and pellets and for total gas--exclusive of moisture--in pellets. Spectrochemical methods are described for the determination of rare earths, 36 trace elements whose recommended analytical spectral lines and concentration ranges are tabulated, and impurities occurring in the atom-ppB range

  17. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1999-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets to determine compliance with specifications. 1.2 This test method covers the determination of uranium and the oxygen to uranium atomic ratio in nuclear-grade uranium dioxide powder and pellets. 1.4 This test method covers the determination of chlorine and fluorine in nuclear-grade uranium dioxide. With a 1 to 10-g sample, concentrations of 5 to 200 g/g of chlorine and 1 to 200 μg/g of fluorine are determined without interference. 1.5 This test method covers the determination of moisture in uranium dioxide samples. Detection limits are as low as 10 μg. 1.6 This test method covers the determination of nitride nitrogen in uranium dioxide in the range from 10 to 250 μg. 1.7 This test method covers the spectrographic analysis of nuclear-grade UO2 for the 26 elements in the ranges indicated in Table 2. 1.8 For simultaneous determination of trace ele...

  18. Determination of lithium and potassium in uranium oxide powders and pellets by Flame Atomic Emission Spectrometric method

    International Nuclear Information System (INIS)

    The present paper describes a method developed at Control Laboratory, NFC which includes prior separation of lithium and potassium from uranium matrix before their measurements. Solvent extraction, using Tri-n-Butyl Phosphate (TBP) in CCI4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI4, is employed for prior separation of Li and K. The resultant aqueous solution was analyzed by Flame-Atomic Emission Spectrometric (AES) method. Solvent extraction conditions are optimized for measurement of Li and K in the same aliquot. Experimental conditions such as instrument calibration, flame condition, fuel flow, sample flow rate through nebulizer, burner height etc. are also optimized. Under the optimal condition the detection limits achieved for lithium is 0.02 ppm and 0.2 ppm for potassium. A RSD of ± 3 % for Li at 0.05 ppm and ± 4% for K at 1 ppm level has been achieved in this method. The results of lithium in the sample are compared with the values obtained by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Similarly, values of potassium are compared with Flame-Atomic Absorption Spectrometry (Flame-AAS) technique. The comparisons are in good agreement. The above method is simple, sensitive, reproducible and can be used for measurement of lithium and potassium in UO2 powder and pellets on regular basis

  19. Gas chromatographic-mass spectrometric analysis of volatiles obtained by four different techniques from Salvia rosifolia Sm., and evaluation for biological activity.

    Science.gov (United States)

    Ozek, Gulmira; Demirci, Fatih; Ozek, Temel; Tabanca, Nurhayat; Wedge, David E; Khan, Shabana I; Başer, Kemal Hüsnü Can; Duran, Ahmet; Hamzaoglu, Ergin

    2010-01-29

    Four different isolation techniques, conventional hydrodistillation (HD), microwave-assisted hydrodistillation (MWHD), microdistillation (MD) and micro-steam distillation-solid-phase microextraction (MSD-SPME), have been used to analyze the volatile constituents from the aerial parts of Salvia rosifolia Sm. by gas chromatography and gas chromatography coupled to mass spectrometry. HD and MWHD techniques produced quantitatively (yield, 0.39% and 0.40%) and qualitatively (aromatic profile) similar essential oils. alpha-Pinene (15.7-34.8%), 1,8-cineole (16.6-25.1%), beta-pinene (6.7-13.5%), beta-caryophyllene (1.4-5.0%) and caryophyllene oxide (1.4-4.4%) were identified as major constituents of this Turkish endemic species. Besides, the hydrodistilled oil of S. rosifolia was evaluated for antibacterial, antifungal, anticancer, antioxidant and cytotoxic activities. The hydrodistilled oil of S. rosifolia showed antibacterial activity against Methicillin-resistant Staphylococcus aureus (MRSA) with a MIC value of 125microg/mL. Other human pathogenic microorganisms (Escherichia coli, Pseudomonas aeruginosa, Enterobacter aerogenes, Salmonella typhimurium, Staphylococcus epidermidis, Candida albicans) were also inhibited within a moderate range (MIC=125-1000microg/mL). Antifungal activity of the oil was also observed against the strawberry anthracnose-causing fungal plant pathogens Colletotrichum acutatum, C. fragariae and C. gloeosporioides. No cytotoxicity was observed for S. rosifolia oil up to 25mg/mL against malignant melanoma, epidermal, ductal and ovary carcinoma. PMID:20015509

  20. A review of recent advances in mass spectrometric methods for gas-phase chiral analysis of pharmaceutical and biological compounds.

    Science.gov (United States)

    Wu, Lianming; Vogt, Frederick G

    2012-10-01

    Chirality has been of great interest in pharmaceutical and biological sciences. The capabilities of mass spectrometry (MS) for rapid analysis of complex mixtures have encouraged its exploration for gas-phase chiral differentiation. Although particular instances of successful discrimination between enantiomers have been reported over the past three decades, a general method of quantitative chiral analysis by MS has only been demonstrated recently. This review describes the current state of the chiral MS methods without chiral chromatographic separation, which fall into five main categories: (1) the kinetic method, (2) host-guest (H-G) diastereomeric adduct formation, (3) ion/molecule (equilibrium) reactions, (4) collision-induced dissociation (CID) of diastereomeric adducts, and (5) the emerging technique for gas-phase separation using ion mobility spectrometry (IMS). It emphasizes tandem mass spectrometry (MS/MS), which provides several unique analytical advantages for quantitative chiral analysis. These include intrinsically high sensitivity, molecular specificity, and tolerance to impurities as well as the simplicity and speed of the mass spectrometric measurements. Practical prospects and current challenges in quantitative chiral MS techniques for QbD (quality-by-design)-based pharmaceutical applications are also discussed. PMID:22579598

  1. Differentiation of the Four Major Species of Cinnamons (C. burmannii, C. verum, C. cassia, and C. loureiroi) Using a Flow Injection Mass Spectrometric (FIMS) Fingerprinting Method

    OpenAIRE

    Chen, Pei; Sun, Jianghao; Ford, Paul

    2014-01-01

    A simple and efficient flow injection mass spectrometric (FIMS) method was developed to differentiate cinnamon (Cinnamomum) bark (CB) samples of the four major species (C. burmannii, C. verum, C. aromaticum, and C. loureiroi) of cinnamon. Fifty cinnamon samples collected from China, Vietnam, Indonesia, and Sri Lanka were studied using the developed FIMS fingerprinting method. The FIMS fingerprints of the cinnamon samples were analyzed using principal component analysis (PCA). The FIMS techniq...

  2. Internal standard method in α spectrometric determination of uranium and thorium radioisotopes using instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    A new approach to α spectrometric determination of the radioisotopes of uranium and thorium was developed for environmental samples based on 238U and 232Th as internal standards. 238U and 232Th were accurately determined in the sample by simultaneous instrumental neutron activation analysis. Other aliquots of the sample were totally dissolved, uranium and thorium separated by anion exchange, and thin sources electroplated for α spectrometry. From the known mass concentrations of 238U and 232Th, their activity concentrations were obtained, and thus from the relative ratios of uranium (234U, 235U, 238U) and thorium (228Th, 230Th, 232Th) radioisotopes in the α spectra, the absolute isotopic activity concentrations were derived. The advantages of the procedure are that neither the chemical recovery of the radiochemical separation nor the counting efficiency of the α spectrometer is required; the use of internal standards eliminates the need for addition of expensive, calibrated, external radioisotopic tracers such as 232U and 229Th. The new approach was tested on some certified environmental reference materials and compared with the classical method using external radioisotopic tracers. It may advantageously be combined with the standard approach to obtain an independent set of data for quality control. 25 refs

  3. Interaction of norfloxacin with bovine serum albumin studied by different spectrometric methods; displacement studies, molecular modeling and chemometrics approaches

    Energy Technology Data Exchange (ETDEWEB)

    Naseri, Abdolhossein, E-mail: a_naseri@tabrizu.ac.ir [Departments of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51666-16471 (Iran, Islamic Republic of); Hosseini, Soheila [Departments of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51666-16471 (Iran, Islamic Republic of); Rasoulzadeh, Farzaneh [Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz 51644-14766 (Iran, Islamic Republic of); Rashidi, Mohammad-Reza [Research Center for Pharmaceutical Nanotechnology, Tabriz University of Medical Sciences, Tabriz 51644-14766 (Iran, Islamic Republic of); Zakery, Maryam; Khayamian, Taghi [Department of Chemistry, College of Chemistry, Isfahan University of Technology, Isfahan 84154 (Iran, Islamic Republic of)

    2015-01-15

    Serum albumins as major target proteins can bind to other ligands leading to alteration of their pharmacological properties. The mechanism of interaction between norfloxacin (NFLX) with bovine serum albumin (BSA) was investigated. Fuorescence quenching of serum albumin by this drug was found to be a static quenching process. The binding sites number, n, apparent binding constant, K, and thermodynamic parameters were calculated at different temperatures. The distance, r, between donor, BSA, and acceptor, NFLX, was calculated according to the Forster theory of non-radiation energy transfer. Also binding characteristics of NFLX with BSA together with its displacement from its binding site by kanamycin and effect of common metal ions on binding constant were investigated by the spectroscopic methods. The conformational change in the secondary structure of BSA upon interaction with NFLX was investigated qualitatively from synchronous fluorescence spectra, Fourier Transform Infrared (FTIR) and circular dichroism (CD) spectrometric methods. Molecular docking studies were performed to obtain information on the possible residues involved in the interaction process and changes in accessible surface area of the interacting residues. The results showed that the conformation of BSA changed in the presence of NFLX. For the first time, displacement studies were used for this interaction; displacement studies showed that NFLX was displaced by phenylbutazon and ketoprofen but was not displaced by ibuprofen indicating that the binding site of NFLX on albumin was site I. In addition a powerful chemometrics method, multivariate curve resolution-alternating least square, was used for resolution of spectroscopic augmented data obtained in two different titration modes in order to extract spectral information regardless of spectral overlapping of components. - Highlights: • Interaction between norfloxacin and BSA is studied by spectral methods. • Chemometrics methods are used to

  4. Interaction of norfloxacin with bovine serum albumin studied by different spectrometric methods; displacement studies, molecular modeling and chemometrics approaches

    International Nuclear Information System (INIS)

    Serum albumins as major target proteins can bind to other ligands leading to alteration of their pharmacological properties. The mechanism of interaction between norfloxacin (NFLX) with bovine serum albumin (BSA) was investigated. Fuorescence quenching of serum albumin by this drug was found to be a static quenching process. The binding sites number, n, apparent binding constant, K, and thermodynamic parameters were calculated at different temperatures. The distance, r, between donor, BSA, and acceptor, NFLX, was calculated according to the Forster theory of non-radiation energy transfer. Also binding characteristics of NFLX with BSA together with its displacement from its binding site by kanamycin and effect of common metal ions on binding constant were investigated by the spectroscopic methods. The conformational change in the secondary structure of BSA upon interaction with NFLX was investigated qualitatively from synchronous fluorescence spectra, Fourier Transform Infrared (FTIR) and circular dichroism (CD) spectrometric methods. Molecular docking studies were performed to obtain information on the possible residues involved in the interaction process and changes in accessible surface area of the interacting residues. The results showed that the conformation of BSA changed in the presence of NFLX. For the first time, displacement studies were used for this interaction; displacement studies showed that NFLX was displaced by phenylbutazon and ketoprofen but was not displaced by ibuprofen indicating that the binding site of NFLX on albumin was site I. In addition a powerful chemometrics method, multivariate curve resolution-alternating least square, was used for resolution of spectroscopic augmented data obtained in two different titration modes in order to extract spectral information regardless of spectral overlapping of components. - Highlights: • Interaction between norfloxacin and BSA is studied by spectral methods. • Chemometrics methods are used to

  5. Partial vapor-phase hydrolysis of peptide bonds: A method for mass spectrometric determination of O-glycosylated sites in glycopeptides

    DEFF Research Database (Denmark)

    Mirgorodskaya, E; Hassan, H; Wandall, H H;

    1999-01-01

    resulting mass spectra allowed unambiguous determination of the glycosylation sites. Examples are shown with mannosyl- and mucin-type glycopeptides. Performing the hydrolysis in vapor eliminates the risk for contamination of the sample with impurities from the reagents, thus allowing analysis of the......In this study we present a method for determination of O-glycosylation sites in glycopeptides, based on partial vapor-phase acid hydrolysis in combination with mass spectrometric analysis. Pentafluoropropionic acid and hydrochloric acid were used for the hydrolysis of glycosylated peptides. The...... reaction conditions were optimized for efficient polypeptide backbone cleavages with minimal cleavage of glycosidic bonds. The glycosylated residues were identified by mass spectrometric analysis of the hydrolytic cleavage products. Although glycosidic bonds are partially cleaved under acid hydrolysis, the...

  6. Nasal absorption studies of granisetron in rats using a validated high-performance liquid chromatographic method with mass spectrometric detection.

    Science.gov (United States)

    Woo, Jong Soo

    2007-06-01

    Granisetron is a selective 5-HT3 receptor antagonist that is used therapeutically for the prevention of vomiting and nausea associated with emetogenic cancer chemotherapy. Although forms of the drug are commercially available for intravenous and oral dosage, there is a need for intranasal delivery formulations in specific patient populations in which the use of these dosage forms may be unfeasible and/or inconvenient. A rapid and specific high-performance liq uid chromatography method with mass spectrometric detection (LC-MS) was developed and validated for the analysis of granisetron in plasma after nasal administration in rats. Granisetron was separated in a reverse-phase C-18 column without interference from other components of plasma. This method involves a rapid assay for the determination of granisetron in a small volume of plasma with a run time of 12 min using ondansetron as an internal standard. Data were acquired in the electrospray ionization (ESI) mode with positive ion detection and application of single ion recording (SIR). Granisetron and ondansetron were detected at m/z values of 313.2 and 294.2, respectively. The method described was found to be suitable for the analysis of all samples collected during preclinical pharmacokinetic investigations of granisetron in rats after nasal administration. To date, the first pharmacokinetic study after intranasal administration of granisetron was performed and some pharmacokinetic parameters were presented in this paper. Granisetron was found to be well absorbed through nasal route and the bioavailability of this drug following nasal administration was comparable with that of intravenous administration. PMID:17679558

  7. Spectrometric techniques 2

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume II provides information pertinent to vacuum ultraviolet techniques to complete the demonstration of the diversity of methods available to the spectroscopist interested in the ultraviolet visible and infrared spectral regions. This book discusses the specific aspects of the technique of Fourier transform spectroscopy.Organized into five chapters, this volume begins with an overview of the large number of systematic effects in the recording of an interferogram. This text then examines the design approach for a Fourier transform spectrometer with focus on optics.

  8. A method for the determination of counting efficiencies in γ-spectrometric measurements with HPGe detectors

    International Nuclear Information System (INIS)

    In this paper a general method for γ-ray efficiency calibration is presented. The method takes into account the differences of densities and counting geometry between the real sample and the calibration sample. It is based on the γ-transmission method and gives the correction factor f as a function of Eγ, the density and counting geometry. Altough developed for soil samples, its underlying working philosophy is useful for any sample whose geometry can be adequately reproduced. (orig.)

  9. Method Validation for the Gamma-ray Spectrometric Determination of Natural Radioactive Nuclides in NORM Samples - Method Validation for the Gamma-ray Spectrometric Determination of Natural Radionuclides in raw materials and by-products

    International Nuclear Information System (INIS)

    sample, were introduced for analyzing 235U, 226Ra and 238U using a HPGe detector. Their results were compared with 235U and 238U from the alpha spectrometer as well as the ICP-MS for the same samples. As a result, the most suitable method of choice can be selected to make gamma-ray spectrometric determination of natural radionuclides as considering an accuracy and time and cost constraints. Finally, a selected method was used to analyze the radioactive inventory in NORM samples and the radioactive equilibrium or disequilibrium state for 238U and 226Ra. (authors)

  10. Development of Mass Spectrometric Ionization Methods for Fullerenes and Fullerene Derivatives

    Science.gov (United States)

    Currently investigations into the environmental behavior of fullerenes and fullerene derivatives is hampered by the lack of well characterized standards and by the lack of readily available quantitative analytical methods. Reported herein are investigations into the utility of ma...

  11. Radon tightness of different sample sealing methods for gamma spectrometric measurements of 226Ra

    International Nuclear Information System (INIS)

    Different methods for sealing sample containers for 222Rn when measuring 226Ra through its progenies 214Pb and 214Bi using gamma-ray spectrometry have been investigated. Results show that a method consisting of vacuum packaging of the sample container in a sealed aluminium lined bag gives excellent results for ensuring radon tightness. However, care should be taken to fill the sample container completely in order to avoid systematic errors due to radon accumulating in the void volume. - Highlights: • Simple and practical sample container sealing methods for 222Rn have been studied. • A novel vacuum packaging method is accurate, practical and cost-effective. • Void volumes in the container should be avoided to prevent systematic influences

  12. Spectrometric Methods Used to Determine Heavy Metals and Total Cyanides in Accidental Polluted Soils

    OpenAIRE

    A. Mihaly-Cozmuta; L. M. Cozmuta; V. Viman; Gh. Vatca; Varga, C.

    2005-01-01

    The study presents the level of soil pollution in the area adjacent to three sedimentation ponds as a result of an environmental accident. Soil samples from various sites have been collected and analyzed to determine the concentration of heavy metals (Cu, Pb, Zn) and total cyanides. The analysis methods used were ICP-AES for heavy metals and the colorimetric for total cyanides. The accuracy of both methods is determined subject to the reproducibility of the results. The values of determined c...

  13. Development of a Mass Spectrometric Method for Pharmacokinetic Study of Trastuzumab

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Nam Young; Choi, Jin Nyoung; Kang, Jeong Won; Choi, Do Young; Kim, Kwang Pyo [Kyung Hee Univ., Yongin (Korea, Republic of); Park, Gyutae [CKD Research Institute, Yongin (Korea, Republic of)

    2014-06-15

    The HPLC-MS/MS method described here is a simple, rapid and specific method for determining the concentration of biologics in mouse serum. This method was validated for the quantification trastuzumab in ICR mice serum. Although the ELISA method is available for the pharmacokinetics study for trastuzumab, but these methods require development of the target specific antibodies. Generally, the development of the target specific antibodies for quantification is time consuming and expensive. In contrast, MRM-based method does not need antibodies for quantification. The therapeutic monoclonal antibody drug Trastuzumab (INN; trade name Herceptin) is widely used for treating metastatic breast cancer patients with overexpression of HER2 on the tumor. Trastuzumab is a representative target therapeutics as a monoclonal antibody that selectively binds with high affinity to the extracellular domain of the human epidermal growth factor receptor 2 protein, HER2. HER2 is amplified or over-expressed in about 20% to 30% of patients with breast cancer and is associated with aggressive disease. Trastuzumab has an inhibitory effect on the overexpression of HER2 receptor, thereby it has been used in treating breast cancer, and also gastric cancer.

  14. Atomic Absorption Spectrometric Method for Estimation of Diclofenac sodium and Mefenamic acid in Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    Sunil Jawla

    2010-01-01

    Full Text Available Diclofenac sodium and Mefenamic acid have been quantified in tablet dosage form by atomic absorption spectrometry (AAS. These methods are based on formation of the metal complexes of Diclofenac sodium and Mefenamic acid with cupric chloride and cobaltous chloride. The first method is based on reaction of both the drugs with cupric chloride to give light blue colored metal complexes, which are then extracted with dichloromethane and digested with 0.1 M nitric acid. Both the drugs are indirectly estimated via determination of copper content in the formed complexes by AAS. The second method is based on the formation of pink colored complexes of both the drugs with cobaltous chloride. These metal complexes are extracted with dichloromethane and estimated via determination of cobalt content in the formed complexes after digestion with 0.1 M nitric acid by AAS.

  15. A Mass Spectrometric Analysis Method Based on PPCA and SVM for Early Detection of Ovarian Cancer

    Directory of Open Access Journals (Sweden)

    Jiang Wu

    2016-01-01

    Full Text Available Background. Surfaced-enhanced laser desorption-ionization-time of flight mass spectrometry (SELDI-TOF-MS technology plays an important role in the early diagnosis of ovarian cancer. However, the raw MS data is highly dimensional and redundant. Therefore, it is necessary to study rapid and accurate detection methods from the massive MS data. Methods. The clinical data set used in the experiments for early cancer detection consisted of 216 SELDI-TOF-MS samples. An MS analysis method based on probabilistic principal components analysis (PPCA and support vector machine (SVM was proposed and applied to the ovarian cancer early classification in the data set. Additionally, by the same data set, we also established a traditional PCA-SVM model. Finally we compared the two models in detection accuracy, specificity, and sensitivity. Results. Using independent training and testing experiments 10 times to evaluate the ovarian cancer detection models, the average prediction accuracy, sensitivity, and specificity of the PCA-SVM model were 83.34%, 82.70%, and 83.88%, respectively. In contrast, those of the PPCA-SVM model were 90.80%, 92.98%, and 88.97%, respectively. Conclusions. The PPCA-SVM model had better detection performance. And the model combined with the SELDI-TOF-MS technology had a prospect in early clinical detection and diagnosis of ovarian cancer.

  16. Combined Electric, Electromagnetic and Gamma Spectrometric Methods Applied to the Pariquera-Açu Alkaline Complex

    Directory of Open Access Journals (Sweden)

    Elaine Maria Lopes Loureiro

    2011-08-01

    Full Text Available The Pariquera-Açu Alkaline Complex, located in the city of Pariquera-Açu (State of São Paulo, is one of the Brazilianalkaline complexes which has considerable mining potential. The combined use of several methods helped to determinepossible areas for exploration. Geophysical prospecting methods were used to assess the exploration potential of theseareas. The methods used in this study were gamma-spectrometry, induced polarization and electrical survey. Previousgeophysical studies were carried out to better understand the structural evolution of the complex and were not limited tothe study of the lithological variation. Gravimetric studies showed a zone of intense fenitization, which is consistent withalkaline complexes with carbonatites. A dipole-dipole survey conducted in the central part of the complex indicated thepresence in the subsurface of a resistive lithology with high chargeability. These factors, together with other studies onthe alkaline complex, suggest the presence of carbonatite in the area, which is corroborated by gamma spectrometry data,given the concentrations of Th (8 ppm and U (3.5 ppm and considering that the measurements were performed over a nonradioactivesedimentary cover.

  17. Comparison of digital methods for storage, sorting and displaying of the spectrometric information

    International Nuclear Information System (INIS)

    During ten years at the Kyiv tandem EGP-10K beam of accelerated hydrogen ions was used extensively in the inclusive and exclusive experiments with scattering and nuclear reactions on different nuclei. Charged particles (protons, deuterons, 4He),γ-quanta and neutrons were registered in the outgoing channels of the studied nuclear processes. This required to use of different methods of radiation spectrometry. The most used (δE x E)-method for spectrometry of charged particles and the time-of-flight method for registration and the separation of neutrons and ?-rays. The current need of the algorithm universalization for measurement and data processing was led to the development, installation and use of computerized multiparameter setup that was used successfully in this time in the beam experiments. This paper discusses the results of the facility modernization in accordance with the development of digital technology, above all, communication devices for measuring apparatus and control computer, and related changes and improves of the operating systems and software for data processing

  18. New method for mass spectrometric trace analysis of metals in biology and medicine

    International Nuclear Information System (INIS)

    A first survey on the basic aspects and applications of a novel method for trace analyses of metals is given. The advantages of this methodology for analyses of trace metals which was developed by our group are: small sample amount, high sensitivity and selectivity, simple sample preparation for the measurement (no ashing) and reliability and precision of the results. The time consumption for one complete quantitative analysis lies below 30 min. The concentration of monoisotopic metals, as for example aluminium, cesium, manganese etc. is determined using a calibration curve. Using stable isotope dilution analysis quantification of metals with at least two stable isotopes further improved the precision of the results. If this technique is utilized, on one hand contamination of the environment by radioactive substances is avoided, on the other even the smallest changes in concentrations of trace metals are detected unambigeously. The accuracy of the resulting quantitative data has been confirmed test measurements with other analytical methods such as atomic absorption spectroscopy and thermal ionization mass spectrometry. Although there is no doubt that the greatest analytical capacity of field desorption mass spectrometry is in the field of high-molecular weight natural products, it has been possible in the last years to modify the method for qualitative and quantitative investigations of more than 60 metals. (orig./EF)

  19. A mass spectrometric method to determine activities of enzymes involved in polyamine catabolism

    Energy Technology Data Exchange (ETDEWEB)

    Moriya, Shunsuke; Iwasaki, Kaori [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan); Samejima, Keijiro, E-mail: samejima-kj@igakuken.or.jp [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan); Takao, Koichi [Faculty of Pharmaceutical Sciences, Josai University, 1-1 Keyakidai, Sakado, Saitama 350-0295 (Japan); Kohda, Kohfuku [Research Institute of Pharmaceutical Sciences, Musashino University, 1-1-20 Shinmachi, Nishitokyo, Tokyo 202-8585 (Japan); Hiramatsu, Kyoko; Kawakita, Masao [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan)

    2012-10-20

    Highlights: Black-Right-Pointing-Pointer Compounds in polyamine catabolic pathway were determined by a column-free ESI-TOF MS. Black-Right-Pointing-Pointer N{sup 1}- and N{sup 8}-acetylspermidine were determined by a column-free ESI-MS/MS. Black-Right-Pointing-Pointer The method was applied to determine activities of APAO, SMO, and SSAT in the pathway. Black-Right-Pointing-Pointer The assay method contained stable isotope-labeled natural substrates. Black-Right-Pointing-Pointer It is applicable to biological samples containing natural substrate and product. - Abstract: An analytical method for the determination of three polyamines (putrescine, spermidine, and spermine) and five acetylpolyamines [N{sup 1}-acetylspermidine (N{sup 1}AcSpd), N{sup 8}-acetylspermidine (N{sup 8}AcSpd), N{sup 1}-acetylspermine, N{sup 1},N{sup 8}-diacetylspermidine, and N{sup 1},N{sup 12}-diacetylspermine] involved in the polyamine catabolic pathway has been developed using a hybrid tandem mass spectrometer. Heptafluorobutyryl (HFB) derivatives of these compounds and respective internal standards labeled with stable isotopes were analyzed simultaneously by TOF MS, based on peak areas appearing at appropriate m/z values. The isomers, N{sup 1}AcSpd and N{sup 8}AcSpd were determined from their fragment ions, the acetylamidopropyl and acetylamidobutyl groups, respectively, using MS/MS with {sup 13}C{sub 2}-N{sup 1}AcSpd and {sup 13}C{sub 2}-N{sup 8}AcSpd which have the {sup 13}C{sub 2}-acetyl group as an internal standard. The TOF MS method was successfully applied to measure the activity of enzymes involved in polyamine catabolic pathways, namely N{sup 1}-acetylpolyamine oxidase (APAO), spermine oxidase (SMO), and spermidine/spermine N{sup 1}-acetyltransferase (SSAT). The following natural substrates and products labeled with stable isotopes considering the application to biological samples were identified; for APAO, [4,9,12-{sup 15}N{sub 3}]-N{sup 1}-acetylspermine and [1,4,8-{sup 15}N{sub 3

  20. Comparison of mass spectrometric methods (TE, MTE and conventional) for uranium isotope ratio measurements

    International Nuclear Information System (INIS)

    The isotope ratio measurement techniques - total evaporation (TE), modified total evaporation (MTE), and conventional - used for characterization measurements of certified reference materials by thermal ionization mass spectrometer instruments are compared. The advantages of each method, the fractionation profiles resulting from the measurement techniques, and factors affecting systematic components of bias in the isotope ratio measurements are discussed. The TE and MTE techniques yield major ratios and the conventional and MTE techniques yield minor ratios of comparable quality (in terms of precision and accuracy). (author)

  1. Characterization and quantification of iodine species in surface waters by radioanalytical and mass spectrometric methods

    International Nuclear Information System (INIS)

    By way of radiochemical labelling experiments, a method was established allowing the extraction of four different iodine species: iodide, iodate, and two organoiodine compounds. The method was a strongly alkaline anion exchanger, to which the four iodine species are bonded with different strenght. The organic radioiodine species were detectable in a 131I-labelled water sample only after it was allowed to stand for a longer period, during which 131I undergoes a transformation which reaches an equilibrium after a period of 14 days. Three iodine species could be eluated, - iodide, iodate, and one anionic organoiodine compound - , while the fourth iodine species remained firmly bonded to the exchanger and was defined as non-elutable organoiodine. Further experiments for characterization were done with membrane filters of different pore size, which allow a fractionation of organic compounds according to molecular weights. The separation of the four iodine species determined by labelling and column chromatography was applied to the quantitative analysis using MS-IVA, and thus for the first time direct determination of iodide, iodate, and anionic organoiodine was achieved. Very different types of surface waters were analysed, and in flowing waters only low amounts of dissolved organic carbon were measured, the different flowing water samples being distinguished primarily by their carbonate concentrations. One boggy water sample, however, contained high concentration of humates (measured as dissolved organic carbon). Every water type was analysed several times and in different seasons of the year. These experiments showed that the various chemical bond types of the iodine are influenced by the prevailing water parameters. (orig./HK)

  2. Preparation of pyrolysis reference samples: evaluation of a standard method using a tube furnace.

    Science.gov (United States)

    Sandercock, P Mark L

    2012-05-01

    A new, simple method for the reproducible creation of pyrolysis products from different materials that may be found at a fire scene is described. A temperature programmable steady-state tube furnace was used to generate pyrolysis products from different substrates, including softwoods, paper, vinyl sheet flooring, and carpet. The temperature profile of the tube furnace was characterized, and the suitability of the method to reproducibly create pyrolysates similar to those found in real fire debris was assessed. The use of this method to create proficiency tests to realistically test an examiner's ability to interpret complex gas chromatograph-mass spectrometric fire debris data, and to create a library of pyrolsates generated from materials commonly found at a fire scene, is demonstrated. PMID:22220974

  3. Synthesis of 4,5,6,7 and 2,4,5,6,7 deuterium-labeled indole-3-acetic acid for use in mass spectrometric assays

    International Nuclear Information System (INIS)

    Syntheses are described for tetra and pentadeutero indole-3-acetic acid (IAA) labeled in positions 4,5,6,7 or 2,4,5,6,7 of the indole moiety. Polydeuterated IAA is proposed as an internal standard for gas chromatographic-mass spectrometric analysis of IAA by selected ion monitoring. Nanogram amounts of IAA may be assayed by monitoring the base peak of IAA at m/z = 130 (134 for d4-IAA) and the molecular ion of the methyl ester of IAA at 189 (193 for d4-IAA). Deuterium in positions 4,5,6, and 7 and, to only a slightly lesser extent, that in position 2 of IAA is retained during alkali treatment, thus permitting use of these compounds as internal standards for assay of IAA released by alkaline hydrolysis of ester and amide conjugates. The use of polydeutero internal standards separates the standards from the isotope cluster caused by the normal abundance of heavy isotopes and also permits use of reduced mass resolution, thus leading to a 10-fold increase in sensitivity. Tetradeutero IAA was used as an internal standard for determining free plus ester IAA in alkaline hydrolysates of Zea mays, and showed exact agreement between estimates based on the molecular ion of the methyl ester and those based upon base peak. Application of the method to measuring free IAA in the upper and lower halves of geotropically stimulated Zea shoots showed 61 +- 4% of the free IAA to be on the lower side

  4. Validation of a method to the addition the multiple standard in the analysis of Pb in reservoir waters for atomic absorption spectrometric

    International Nuclear Information System (INIS)

    The evaluation of a method is presented for the analysis of Pb in reservoir waters for atomic spectrometric with direct aspiration. For the validation of the analytic method a level of concentration of 0.05 mg/L was evaluated. The precision of the method was of 9.97% and the bias was 0.6% 8 samples of surface waters they were collected and of bottom of the tributaries of the reservoir Scorpions and the stocking of the concentrations in the tributaries was from 0,052 +- 0.026 inferior mg/L to the established one in the Cuban norm of evaluation of the hydirc objects of fishing use

  5. Differentiation of the four major species of cinnamons (C. burmannii, C. verum, C. cassia, and C. loureiroi) using a flow injection mass spectrometric (FIMS) fingerprinting method.

    Science.gov (United States)

    Chen, Pei; Sun, Jianghao; Ford, Paul

    2014-03-26

    A simple and efficient flow injection mass spectrometric (FIMS) method was developed to differentiate cinnamon (Cinnamomum) bark (CB) samples of the four major species (C. burmannii, C. verum, C. aromaticum, and C. loureiroi) of cinnamon. Fifty cinnamon samples collected from China, Vietnam, Indonesia, and Sri Lanka were studied using the developed FIMS fingerprinting method. The FIMS fingerprints of the cinnamon samples were analyzed using principal component analysis (PCA). The FIMS technique required only 1 min of analysis time per sample. The representative samples from each of the four major species of cinnamon were further examined using an ultrahigh-performance liquid chromatography-high-resolution mass spectrometry system, and the chemical differences between the four species were profiled. The results showed that the 1 min FIMS fingerprinting method successfully differentiated the four cinnamon species studied. PMID:24628250

  6. A sensitive mass spectrometric method for hypothesis-driven detection of peptide post-translational modifications: multiple reaction monitoring-initiated detection and sequencing (MIDAS).

    Science.gov (United States)

    Unwin, Richard D; Griffiths, John R; Whetton, Anthony D

    2009-01-01

    The application of a targeted mass spectrometric workflow to the sensitive identification of post-translational modifications is described. This protocol employs multiple reaction monitoring (MRM) to search for all putative peptides specifically modified in a target protein. Positive MRMs trigger an MS/MS experiment to confirm the nature and site of the modification. This approach, termed MIDAS (MRM-initiated detection and sequencing), is more sensitive than approaches using neutral loss scanning or precursor ion scanning methodologies, due to a more efficient use of duty cycle along with a decreased background signal associated with MRM. We describe the use of MIDAS for the identification of phosphorylation, with a typical experiment taking just a couple of hours from obtaining a peptide sample. With minor modifications, the MIDAS method can be applied to other protein modifications or unmodified peptides can be used as a MIDAS target. PMID:19444244

  7. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade mixed oxides ((U, Pu)O2)

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade mixed oxides, (U, Pu)O2, powders and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Uranium in the Presence of Pu by Potentiometric Titration Plutonium by Controlled-Potential Coulometry Plutonium by Amperometric Titration with Iron (II) Nitrogen by Distillation Spectrophotometry Using Nessler Reagent 7 to 14 Carbon (Total) by Direct Combustion-Thermal Conductivity 15 to 26 Total Chlorine and Fluorine by Pyrohydrolysis 27 to 34 Sulfur by Distillation-Spectrophotometry 35 to 43 Moisture by the Coulometric, Electrolytic Moisture Analyzer 44 to 51 Isotopic Composition by Mass Spectrometry Rare Earths by Copper Spark Spectroscopy 52 to 59 Trace Impurities by Carrier Distillation Spectroscopy 60 to 69 Impurities by Spark-Source Mass Spectrography 70 to 76 Total Gas in Reactor-Grade Mixed Dioxide P...

  8. Development of a coupled-column liquid chromatographic-tandem mass spectrometric method for the direct determination of betamethasone in urine.

    Science.gov (United States)

    Polettini, A; Marrubini Bouland, G; Montagna, M

    1998-08-25

    Different hyphenated liquid chromatographic (LC) and mass spectrometric (MS) techniques were investigated in order to set-up a method for the fast, direct analysis of betamethasone in hydrolysed and non-hydrolysed urine using large-volume sample injection. After the optimisation of the LC parameters using a traditional UV detector and of the thermospray and mass spectrometric parameters by flow injection, urine samples (0.5 ml) were submitted to analysis by either LC combined with tandem mass spectrometry (MS-MS), coupled-column LC (LC-LC) combined with single quadrupole MS, and LC-LC-MS-MS. Both the three-step configurations (LC-MS-MS and LC-LC-MS) did not provide satisfactory results: loss of sensitivity was noted in the case of LC-MS-MS (likely due to reduced efficiency in the ionisation of betamethasone in the thermospray owing to the presence of large amounts of matrix interference), while in the case of LC-LC-MS a high chemical noise resulting in insufficient selectivity of detection was observed. On the contrary, LC-LC-MS-MS analysis proved to meet the demand of high speed of analysis (sample throughput, 4.5 h(-1)), selectivity, and sensitivity (LOQ, 1 ng/ml; LOD, 0.2 ng/ml). Notwithstanding the complex analytical system adopted, the developed procedure was manageable and very robust, provided that at the beginning of each analytical session the performance of the system was controlled by checking the retention time of the analytes on the first analytical column with UV detection and by optimising vaporiser temperature of the thermospray by flow injection. PMID:9746249

  9. Qualification and application of a liquid chromatography-quadrupole time-of-flight mass spectrometric method for the determination of trastuzumab in rat plasma.

    Science.gov (United States)

    Park, Min-Ho; Lee, Min-Woo; Shin, Young G

    2016-04-01

    An liquid chromatography-quadrupole time-of-flight (QqTOF) mass spectrometric method was developed for the determination of humanized or human monoclonal antibodies in rat plasma at the early drug discovery stage. Trastuzumab was used as a model monoclonal antibody. The method consisted of immunoprecipitation followed by tryptic digestion for sample preparation and LC-TOF-MS/MS analysis of specific signature peptides in the positive ion mode using electrospray ionization for analysis. A stable isotope-labeled signature peptide was also used as internal standard. A quadratic regression (weighted 1/concentration(2) ), with an equation y = ax(2)  + bx + c, was used to fit calibration curves over the concentration range of 0.500-100 µg/mL for trastuzumab. Samples from a pharmacokinetic study in rat were analyzed by this qualified LC-TOF-MS/MS method and concentrations were compared with those generated by enzyme linked immunosorbent assays method. The LC-TOF-MS/MS method was accurate and precise, with quantitative results comparable with those of ELISA. The qualification run met the acceptance criteria of ±25% accuracy and precision values for quality control samples. Within-run accuracy ranged from 1.53 to 9.20% with precision values ≤10.29%. This LC-TOF-MS/MS method approach could be used as a complementary method for humanized or human monoclonal antibodies at the early drug discovery stage. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26317190

  10. Spectrometric techniques 3

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  11. A liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric method for the determination of organosulfur compounds in petroleum asphalt cements.

    Science.gov (United States)

    da Silveira, Géssica Domingos; Faccin, Henrique; Claussen, Luis; Goularte, Rayane Bueno; Do Nascimento, Paulo C; Bohrer, Denise; Cravo, Margareth; Leite, Leni F M; de Carvalho, Leandro Machado

    2016-07-29

    We present a sensitive liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (UHPLC-APPI-MS/MS) method for the determination of selected organosulfur compounds in Brazilian asphalt cements. It was possible to detect 14 organosulfur compounds of different classes where sulfoxides and sulfones presented higher sensibility in ionization than thiophenes and aromatic sulfides. A dopant-assisted APPI method was also tested, however, when chromatographic flow rate was optimized a decrease in signal was observed for all compounds. PAHs were tested and ruled out as possible interfering compounds and the matrix effect of asphalt cements was within an acceptable range for the quantification of organosulfur compounds. The proposed method was found to have satisfactory linearity and accuracy with recoveries between 83.85 and 110.28% for thianaphthene and 3-methylbenzothiophene, respectively. Therefore, the method allowed the characterization of organosulfur compounds in Brazilian asphalt cements and demonstrated changes in the amount quantified in asphaltenic and maltenic fractions after the RTFOT+SUNTEST aging process. PMID:27342135

  12. A method of test for residual isophorone diisocyanate trimer in new polyester-polyurethane coatings on light metal packaging using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Driffield, Malcolm; Bradley, Emma L; Castle, Laurence

    2007-02-01

    A method of test for residual isophorone diisocyanate (IPDI) trimer in experimental formulation polyester-polyurethane (PEPU) thermoset coatings on metal food packaging is described. The method involves extraction of coated panels using acetonitrile containing dibutylamine for concurrent derivatisation, and then high performance liquid chromatography with electrospray ionisation tandem mass spectrometric detection (LC-MS/MS). Single laboratory validation was carried out using three different experimental PEPU-based coatings. The calibrations were linear, the analytical recovery was good, no interferences were seen, and substance identification criteria were met. The detection limit of the method is around 0.02 micro g/100 cm(2) of coating, which for a typical sized can and assuming complete migration of any residual IPDI trimer, corresponds to about 0.2 micro g/kg food or beverage. Separate studies indicated that, even if migration occurred at such low levels, the IPDI trimer would not be expected to persist in canned aqueous or fatty foodstuffs as it would hydrolyse to the corresponding aliphatic amine or react with food components to destroy the isocyanate moiety. The method of test developed here for residual IPDI trimer in thermoset polyester-polyurethane coatings should prove to be a valuable tool for investigating the cure kinetics of these novel coatings and help to guide the development of enhanced formulations. PMID:17178416

  13. Analyses of Heavy Metal Contents in the Bulk Atmospheric Aerosols Simultaneously Collected at Okinawa Archipelago, Japan by Using X-ray fluorescence spectrometric method (XRF)

    Science.gov (United States)

    Oshiro, Y.; ITOH, A.; Azechi, S.; Somada, Y.; Handa, D.; Miyagi, Y.; Arakaki, T.; Tanahara, A.

    2012-12-01

    We studied heavy metal contents of bulk atmospheric aerosols using an X-ray fluorescence spectrometric method (XRF). The XRF method enables us to analyze heavy metal contents in the bulk aerosols rapidly without any chemical pretreatments. We used an energy dispersive X-ray fluorescence spectrometer that is compact and portable. We prepared several different amounts of standard reference materials (referred to "SRM", NIES No.28 of Japanese National Institute of Environmental Studies) on quartz filters for calibration curves in two different methods; 1) water-insoluble materials were collected after dispersing SRM in pure water and filtered with the quartz filters ("wet method"), and 2) SRM was dispersed in air in the plastic container and the aerosols were collected by using the low-volume air sampler ("dry method"). Good linear relationships between X-ray intensity and amount of aerosols on the filter were seen in the following 9 metals; Al, K, Ti, V, Fe, Ni, Rb, Ba, and Pb (with wet method) and 12 metals; K, Ti, Fe, Ni, Rb, Ba, Pb, Sr, Ca, Mn, Zn, and Cu (with dry method). Furthermore, we evaluated quantitative responses of XRF method by comparing with the metal contents determined by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after acid-digestion. We then used XRF method to determine heavy metal contents in authentic atmospheric aerosols collected in Okinawa islands, Japan. We simultaneously collected bulk aerosol samples by using identical high-volume air samplers at 3 islands; Cape Hedo Atmospheric Aerosol Monitoring Station (CHAAMS, Okinawa island), Kume island (ca. 160 km south-west of CHAAMS), and Minami-Daitou island (ca. 320 km south-east of CHAAMS). We report and discuss spatial and temporal distribution of heavy metals determined by the XRF method in the bulk atmospheric aerosols collected at the three islands during June 2008 to June 2010, and for CHAAMS during June 2008 to October 2012.

  14. Liquid chromatography-tandem mass spectrometric methods for the determination of spinosad, thiacloprid and pyridalyl in spring onions and estimation of their pre-harvest interval values.

    Science.gov (United States)

    Dasenaki, Marilena E; Bletsou, Anna A; Hanafi, Ahmad H; Thomaidis, Nikolaos S

    2016-12-15

    Two liquid chromatography-tandem mass spectrometric methods were developed and validated to determine spinosyn A and D, thiacloprid and pyridalyl in spring onions cultivated under Egyptian field conditions. The degradation rates, the pre-harvest interval (PHI) values and the half-life values of the three pesticides were estimated. QuEChERS was used for sample preparation and the separation was performed on an X-Bridge C18 column with ACN-formic acid 0.1% as the mobile phase. Linear range, method detection limits (MDLs), precision, recovery and matrix effects were estimated. The multi-residue MDLs ranged from 0.02μg/kg (spinosyn A & D) to 0.05μg/kg for pyridalyl. All the investigated pesticides showed high degradation rates. For spinosad the half-life value was 1.2days, for thiacloprid it reached 2.2days and for pyridalyl 4.4days. Furthermore, the calculated PHI values, according to the maximum residue levels set by the EU, were 0days for spinosad, 9.8days for thiacloprid and 39.4days for pyridalyl. PMID:27451196

  15. Quantitative analysis of sodium di-uranate for Al, Ca, Fe, Mg, Mn, Na by flame-atomic absorption spectrometric method

    International Nuclear Information System (INIS)

    Nuclear Fuel Complex (NFC) receives Sodium Di-Uranate (SDU) from Uranium Corporation of India Limited (UCIL) for producing sinterable UO2 pellets for manufacturing fuel sub assemblies. Several impurities present in ore find their way into SDU during its conversion. Stringent specification have been laid down by the reactor designs for achieving the optimum performance of the fuel and several impurity element like Al, Ca, Fe, Mg, Mn, Na among others affects severely performance of UO2 fuel. Most of the impurity including the above mentioned elements are generally analysed by ICP-OES method. However, determination of Al, Ca, Fe, Mg, Mn and Na by ICP-OES requires lot of dilution as they are present at high levels in SDU. Apart from introducing dilution error, dilution process is very tedious and time consuming work and not a preferred choice in an industrial lab like control lab where large analytical load exists and time bound analysis is a requirement. To avoid these difficulties a simple and reliable Flame Atomic absorption spectrometric technique has been developed for regular analysis. Present method involves dissolution of SDU sample in Conc. HNO3 and after the complete dissolution the sample solution has been evaporated to near dryness on a hot plate. Subsequently sample solution has been brought into 4N HNO3 medium

  16. Application of MnO2 coated disks in the case of the measurement of 226Ra with Alfa-spectrometric method

    International Nuclear Information System (INIS)

    226Ra is a member of the 238U natural decay series, it can be detected by direct - via its α-particle or γ-ray emission, and by indirect methods - via its progenies. The γ-spectrometric and the indirect method are popular, although radioactive equilibrium is required. The α-particle spectrometry is a direct method, and therefore it is not necessary to await the equilibrium of 226Ra with its daughters, and it has high sensitivity, which allow to measure low activity concentrations. It has been reported by several investigators that the MnO2 coated manganese fibres can be used to pre-concentrate radionuclides from large water samples. Polyamide has an ion exchange property by itself; therefore investigators applied MnO2 coated polyamide disks for source preparation. In this work the feasibility of the detection of 226Ra in this introduced way with a semi-conductor PIPS detector were measured, the applied source preparation method based on the 226Ra sorption of on MnO2 coated disks. Circumstances of this source preparation method were measured, and efforts were made to solve the incidental problems. The executed experiments were showed that the method can be applied to detection of 226Ra, however the resolution was weak. It can be caused by the surface roughness and by the width the MnO2 coat. Whereas the surface roughness of MnO2 cannot be changed more, smooth surfaces could produce in another way, so there were took several surfaces into account, like stainless-steel, nickel, copper and chrome plate. (author)

  17. On the fast response of spectrometric circuits

    International Nuclear Information System (INIS)

    Information capacity of spectrometric circuits obtianed by means of Monte Carlo method modeling is analysed. It is shown that working at high input pulse counting rate is not advisable, dead time of analog-to-digital converter should be compared with the pulse rise time of the amplifier

  18. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade aluminum oxide and aluminum oxide-boron carbide composite pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1994-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade aluminum oxide and aluminum oxide-boron carbide composite pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Boron by Titrimetry 7 to 13 Separation of Boron for Mass Spectrometry 14 to 19 Isotopic Composition by Mass Spectrometry 20 to 23 Separation of Halides by Pyrohydrolysis 24 to 27 Fluoride by Ion-Selective Electrode 28 to 30 Chloride, Bromide, and Iodide by Amperometric Microtitrimetry 31 to 33 Trace Elements by Emission Spectroscopy 34 to 46 1.3 The values stated in SI units are to be regarded as the standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. (F...

  19. Development of a high-speed MALDI-triple quadrupole mass spectrometric method for the determination of 3,4-methylenedioxymethamphetamine (MDMA) in oral fluid.

    Science.gov (United States)

    Poetzsch, Michael; Steuer, Andrea E; Hysek, Cedric M; Liechti, Matthias E; Kraemer, Thomas

    2016-02-01

    3,4-Methylenedioxymethamphetamine (MDMA, ecstasy) is still a widely used illicit designer drug and its detection in different matrices is of major importance for forensic purposes (e.g. driving under the influence) as well as for workplace drug testing or abstinence control. Established analytical methods for the determination of MDMA are mainly employing high performance liquid chromatography (HPLC) or gas chromatography (GC) coupled to mass spectrometric detection. Matrix assisted laser desorption/ionization-triple quadrupole-tandem mass spectrometry (MALDI-QqQ-MS/MS) is so far rarely used in forensics and offers an ultrafast high-throughput platform. The Quantisal™ Oral Fluid Collection Device was used for sample collection. After addition of the deuterated internal standard and a carbonate buffer (0.75 M Na2 CO3 ), oral fluid samples were liquid-liquid extracted (ButOAc/EtOAc, 1:1). As little as 1 microlitre of a mixture of this extract and the MALDI matrix (alpha-cyano-4-hydroxycinnamic acid) was spotted onto the MALDI plate and could directly be analyzed. With MALDI omitting chromatographic separation, very short analysis times of about 10 s per sample were possible. The method was developed and validated according to international guidelines including specificity, recovery, matrix effects, accuracy and precision, stabilities and limit of quantification. All validation criteria were fulfilled except for ion suppression/enhancement. Comparison with a routine liquid chromatography-tandem mass spectrometry (LC-MS/MS) method showed good agreement of the results. Applicability of the method was shown by analyzing about 250 oral fluid samples collected after controlled administration of 125 mg MDMA in a pharmacokinetic study. The whole lot of samples could be analyzed in less than 1 h, proving the ultra-high-speed of the method. PMID:25990956

  20. Standard methods for chemical, mass spectrometric, and spectrochemical analysis of, and physical tests on, beryllium oxide powder

    International Nuclear Information System (INIS)

    Methods are described for the determination of C, Fe, N, Cl-, Li, S, thirty trace elements, and the amount of BeO in BeO powder. Methods are included for certain physical properties of the oxide powders. C is determined by the combustion-thermal conductivity method. A colorimetric method using orthophenanthroline is used for the determination of Fe, and N is determined by a micro Kjeldahl method. Chlorine is determined nephlometrically using AgNO3, and Li is determined by atomic absorption spectrophotometry. A complete burning spectrochemical method and a spark-source mass spectrographic method were used to analyze for the thirty trace elements. The density of the BeO powders was measured by a toluene displacement method, and a tap-pak volumetric method was used for the determination of the pour and tap densities. Two different methods described for the particle-size composition determination are Coulter Counter method and sieve analysis method. Methods for determination of bulk density, real density, porosity, and pore size of the solid oxides are described. A nitrogen absorption method is described for the determination of surface area

  1. Determination of Antimycin-A in water by liquid chromatographic/mass spectrometry: single-laboratory validation

    Science.gov (United States)

    Bernardy, Jeffry A.; Hubert, Terrance D.; Ogorek, Jacob M.; Schmidt, Larry J.

    2013-01-01

    An LC/MS method was developed and validated for the quantitative determination and confirmation of antimycin-A (ANT-A) in water from lakes or streams. Three different water sample volumes (25, 50, and 250 mL) were evaluated. ANT-A was stabilized in the field by immediately extracting it from water into anhydrous acetone using SPE. The stabilized concentrated samples were then transported to a laboratory and analyzed by LC/MS using negative electrospray ionization. The method was determined to have adequate accuracy (78 to 113% recovery), precision (0.77 to 7.5% RSD with samples ≥500 ng/L and 4.8 to 17% RSD with samples ≤100 ng/L), linearity, and robustness over an LOQ range from 8 to 51 600 ng/L.

  2. A liquid chromatography-tandem mass spectrometric method for quantitative determination of native 5-methyltetrahydrofolate and its polyglutamyl derivatives in raw vegetables.

    Science.gov (United States)

    Wang, Chao; Riedl, Ken M; Schwartz, Steven J

    2010-11-01

    Folate deficiency is a prevalent phenomenon worldwide especially in underprivileged countries. Polyglutamyl 5-methyltetrahydrofolate (5MTHF) species are the naturally occurring principle folate in store-bought vegetables. Here we report a simple and complete extraction method for the determination of native polyglutamyl 5-methyltetrahydrofolate in vegetables using high performance liquid chromatography with tandem mass spectrometric detection (HPLC-MS/MS). Coarsely chopped samples (18 different vegetables) were steamed to inactivate glutamylase enzymes and liberate folate from binding proteins and extracted in a reducing buffer with (13)C(5) 5MTHF stable isotope added as internal standard. The polyglutamyl 5-methyltetrahydrofolate species were separated in 9 min on a C(18) column using a reversed phase system. HPLC eluate was interfaced with a triple quadrupole mass spectrometer operated in electrospray positive mode. The respective pseudomolecular cation of each polyglutamyl 5-methyltetrahydrofolate species was selected for fragmentation to a common daughter ion for detection. We quantitated polyglutamyl 5-methyltetrahydrofolate in store-bought vegetables from families Brassicaceae, Asteraceae and Amaranthaceae (including mustard greens, romaine lettuce and Swiss chard) of which most have not been quantitated previously. Most vegetables from Asteraceae and those from Amaranthaceae contained similar amounts of monoglutamyl 5MTHF and polyglutamyl 5MTHF while Brassicaceae were dominated by polyglutamyls and endive species (Asteraceae) contained mainly monoglutamyl 5MTHF. The precision of the method for the various polyglutamyl 5-methyltetrahydrofolate forms was 1-9% RSD, recovery 84-91%, limit of detection 64-658 fmol and limit of quantitation 193-1994 fmol. Herein we describe a rapid, sensitive and selective HPLC-MS/MS technique to quantitate polyglutamyl 5-methyltetrahydrofolate species. This method may be suitable for analyzing the polyglutamyl 5

  3. Gas chromatographic-mass spectroscopic determination of benzene in indoor air during the use of biomass fuels in cooking time.

    Science.gov (United States)

    Sinha, Sukesh Narayan; Kulkarni, P K; Desai, N M; Shah, S H; Patel, G M; Mansuri, M M; Parikh, D J; Saiyed, H N

    2005-02-18

    A gas chromatography-mass spectroscopic method in electron ionization (EI) mode with MS/MS ion preparation using helium at flow rate 1 ml min(-1) as carrier gas on DB-5 capillary column (30 m x 0.25 mm i.d. film thickness 0.25 microm) has been developed for the determination of benzene in indoor air. The detection limit for benzene was 0.002 microg ml(-1) with S/N: 4 (S: 66, N: 14). The benzene concentration for cooks during cooking time in indoor kitchen using dung fuel was 114.1 microg m(-3) while it was 6.6 microg m(-3) for open type kitchen. The benzene concentration was significantly higher (p chemist dealing with GC-MS in confirmation and quantification of benzene in environmental samples with health risk exposure assessment. PMID:15782977

  4. Oral and topical pharmacokinetic studies of a novel TRPV1 antagonist, PAC-14028 in rats and minipigs using liquid chromatography/tandem mass spectrometric method.

    Science.gov (United States)

    Park, Yang-Hui; Joo, Kyung-Mi; Woo, Byoung-Young; Son, Eui Dong; Byun, Sang Yo; Shin, Hong-Ju; Lee, Ki-Wha; Park, Young-Ho; Lim, Kyung-Min

    2012-03-01

    PAC-14028 ((E)-N-((R)-1-(3,5-difluoro-4-methanesulfonylamino-phenyl)-ethyl)-3-(2-propyl-6-trifluoromethyl-pyridine-3-yl)-acrylamide) is a novel and potent transient receptor potential vanilloid type I (TRPV1) antagonist. We developed and validated a rapid, sensitive and selective liquid chromatography/tandem mass spectrometric method for determination of PAC-14028 in rat and minipig plasma. After protein precipitation PAC-14028 and internal standard (methylated analog, PAC-14026) were separated on a Symmetry C(18) column (4.6 mm × 75 mm, 3.5 μm) with an isocratic mobile phase, acetonitrile: water (8:2, v/v) containing 0.2% formic acid and monitored by electrospray positive ionization with multiple reaction monitoring mode (PAC-14028, 492→156; IS, 506→156, m/z). The calibration curve was linear over the range of 1.0-500 ng/ml (r(2)>0.999) and lower limit of quantitation (LLOQ) was 1 ng/ml. The precision and accuracy were within ± 15% and the stability was acceptable during bench-top, auto-sampler, 3 freeze-thaw cycles and 4-week storage in a freezer at -80°C. This method was successfully applied to the intravenous, oral and topical pharmacokinetic studies of PAC-14028 in rats and minipigs, which showed comparable pharmacokinetic parameters (T1/2, 2.1h and 3.8h; F%, 52.7% and 64.2% for rats and minipigs, respectively). Percutaneous absorption of PAC-14028 was negligible after topical application (F% 0.2-1.7%). PMID:22169466

  5. Determination of total lead in 400 lipsticks on the U.S. market using a validated microwave-assisted digestion, inductively coupled plasma-mass spectrometric method.

    Science.gov (United States)

    Hepp, Nancy M

    2012-01-01

    In 2009, the U.S. Food and Drug Administration (FDA) published lead (Pb) content results from a small survey of 20 tube lipsticks with red shades using a validated inductively coupled plasma-mass spectrometric (ICP-MS) method developed by FDA chemists. The study was prompted by a media report suggesting that potential exposure to lead from lipsticks under conditions of ordinary use might be harmful. The FDA has since investigated the lead content of tube lipsticks by conducting an expanded survey that included a variety of shades and manufacturers, at varying prices. The purposes of the expanded survey were to ascertain the levels of lead in lipsticks sold on the U.S. market, to identify any categories of lipstick with elevated levels of lead, and to compare the results to those from the initial small survey. Four hundred lipsticks available on the U.S. market in the spring of 2010 were tested for total lead content using the FDA's validated method. The analyses were performed by a private laboratory contracted by the FDA. The maximum lead level found was 7.19 mg Pb/kg. Thirteen of the 400 lipsticks were found to contain levels greater than 3.06 mg Pb/kg, the highest amount found in the initial survey. The average lead concentration found in the expanded survey was 1.11 mg Pb/kg, which was very close to the average of 1.07 mg Pb/kg found in the initial survey. Some statistically significant associations between lead level and parent company were found. The contract requirements, testing procedures, and findings from the expanded survey are described here. PMID:23193690

  6. A liquid chromatography-mass spectrometric method for the detection of cyclic β-amino fatty acid lipopeptides.

    Science.gov (United States)

    Urajová, Petra; Hájek, Jan; Wahlsten, Matti; Jokela, Jouni; Galica, Tomáš; Fewer, David P; Kust, Andreja; Zapomělová-Kozlíková, Eliška; Delawská, Kateřina; Sivonen, Kaarina; Kopecký, Jiří; Hrouzek, Pavel

    2016-03-18

    Bacterial lipopeptides, which contain β-amino fatty acids, are an abundant group of bacterial secondary metabolites exhibiting antifungal and/or cytotoxic properties. Here we have developed an LC-HRMS/MS method for the selective detection of β-amino fatty acid containing cyclic lipopeptides. The method was optimized using the lipopeptides iturin A and puwainaphycin F, which contain fatty acids of similar length but differ in the amino acid composition of the peptide cycle. Fragmentation energies of 10-55eV were used to obtain the amino acid composition of the peptide macrocycle. However, fragmentation energies of 90-130eV were used to obtain an intense fragment specific for the β-amino fatty acid (CnH2n+2N(+)). The method allowed the number of carbons and consequently the length of the β-amino fatty acid to be estimated. We identified 21 puwainaphycin variants differing in fatty acid chain in the crude extract of cyanobacterium Cylindrospermum alatosporum using this method. Analogously 11 iturin A variants were detected. The retention time of the lipopeptide variants showed a near perfect linear dependence (R(2)=0.9995) on the length of the fatty acid chain in linear separation gradient which simplified the detection of minor variants. We used the method to screen 240 cyanobacterial strains and identified lipopeptides from 8 strains. The HPLC-HRMS/MS method developed here provides a rapid and easy way to detecting novel variants of cyclic lipopeptides. PMID:26893022

  7. A high-performance liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric method for determination of risperidone and 9-hydroxyrisperidone in human plasma.

    Science.gov (United States)

    Moody, David E; Laycock, John D; Huang, Wei; Foltz, Rodger L

    2004-09-01

    Risperidone, a benzisoxazole derivative, is an antipsychotic agent used for the treatment of schizophrenia. We developed a liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric (LC-APCI-MS-MS) method with improved sensitivity, selectivity, and dynamic range for determination of risperidone and 9-hydroxyrisperidone in human plasma. A structural analogue of risperidone, RO68808 (5 ng/mL), is added as the internal standard to 1 mL of human plasma. Plasma is made basic, extracted with pentane/methylene chloride (3:1), the organic phase evaporated to dryness, and the residue is reconstituted in water with 0.1% formic acid/acetonitrile (20:1). For LC-MS-MS analysis, a Metachem Inertsel HPLC column (2.1 x 150 mm, 5-microm particle size) is connected to a Finnigan TSQ7000 tandem MS via the Finnigan API interface. Both electrospray (ESI) and APCI produced predominantly MH(+) ions for the two analytes and the internal standard. Ions detected by selected reaction monitoring correspond to the following transitions: m/z 411 to 191 for risperidone, m/z 427 to 207 for 9-hydroxyrisperidone, and m/z 421 to 201 for the internal standard. APCI provided a larger dynamic range (0.1 to 25 ng/mL) and better precision and accuracy than ESI. Intrarun accuracy and precision determined at 0.1, 0.25, 2.5, and 15 ng/mL were within 12% of target with %CVs not exceeding 10.9%. Interrun accuracy and precision determined at the same concentrations were within 9.6% of target with %CVs not exceeding 6.7%. Analytes were stable in plasma after 24 h at room temperature, 2 freeze-thaw cycles, and 490 days at -20 degrees C. PMID:15516302

  8. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Roos, Per

    2008-01-01

    application in the environmental and biological researches, these radionuclides include H-3, C-14, Cl-36, Ca-41 Ni-59,Ni-63, Sr-89,Sr-90, Tc-99, I-129, Cs-135,Cs-137, Pb-210, Ra-226,Ra-228, Np-237, Am-241, and isotopes of thorium, uranium and plutonium. The application of on-line methods (flow injection...

  9. Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

  10. Development of a matrix-assisted laser desorption ionization mass spectrometric method for rapid process-monitoring of phthalocyanine compounds

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Yi-Ting, E-mail: ytchen@mail.cgu.edu.tw [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Molecular Medicine Research Center, College of Medicine, Chang Gung University, Taoyuan 33302, Taiwan (China); Wang, Fu-Shing [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Li, Zhendong [Department of Chemistry, University of Alberta, Alberta T6G 2G2 (Canada); Li Liang, E-mail: liang.li@ualberta.ca [Department of Chemistry, University of Alberta, Alberta T6G 2G2 (Canada); Ling, Yong-Chien, E-mail: ycling@mx.nthu.edu.tw [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

    2012-07-29

    Highlights: Black-Right-Pointing-Pointer MALDI TOFMS is developed as a rapid means of monitoring the process of phthalocyanine derivatives. Black-Right-Pointing-Pointer All-trans retinoic acid is used as matrix to reduce ion fragmentation and background formation. Black-Right-Pointing-Pointer Samples from the reaction process are taken for direct analysis by MALDI TOFMS without any cleanup. Black-Right-Pointing-Pointer The method is demonstrated for monitoring the synthesis of brominated Ni- and Cu-phthalocyanine. - Abstract: Phthalocyanines (PCs), an important class of chemicals widely used in many industrial sectors, are macrocyclic compounds possessing a heteroaromatic {pi}-electron system with optical properties influenced by chemical structures and impurities or by-products introduced during the synthesis process. Analytical tools allowing for rapid monitoring of the synthesis processes are of significance for the development of new PCs with improved performance in many application areas. In this work, we report a matrix-assisted laser desorption/ionization (MALDI) time-of-flight mass spectrometry (TOFMS) method for rapid and convenient monitoring of PC synthesis reactions. For this class of compounds, intact molecular ions could be detected by MALDI using retinoic acid as matrix. It was shown that relative quantification results of two PC compounds could be generated by MALDI MS. This method was applied to monitor the bromination reactions of nickel- and copper-containing PCs. It was demonstrated that, compared to the traditional UV-visible method, the MALDI MS method offers the advantage of higher sensitivity while providing chemical species and relative quantification information on the reactants and products, which are crucial to process monitoring.

  11. Development and application of mass-spectrometric methods for the quantification and characterization of organic compounds in ice cores

    OpenAIRE

    Müller-Tautges, Christina

    2014-01-01

    Eisbohrkerne stellen wertvolle Klimaarchive dar, da sie atmosphärisches Aerosol konservieren. Die Analyse chemischer Verbindungen als Bestandteil atmosphärischer Aerosole in Eisbohrkernen liefert wichtige Informationen über Umweltbedingungen und Klima der Vergangenheit. Zur Untersuchung der α-Dicarbonyle Glyoxal und Methylglyoxal in Eis- und Schneeproben wurde eine neue, sensitive Methode entwickelt, die die Stir Bar Sorptive Extraction (SBSE) mit der Hochleistungsflüssigchromatographie-Masse...

  12. A robust and rapid liquid chromatography tandem mass spectrometric method for the quantitative analysis of 5-azacytidine

    OpenAIRE

    Anders, Nicole M.; Wanjiku, Teresia M.; He, Ping; Azad, Nilofer S.; Rudek, Michelle A.

    2015-01-01

    The DNA methyltransferase inhibitor 5-azacytidine is being evaluated clinically as an oral formulation to treat various solid tumors. A sensitive, reliable method was developed to quantitate 5-azacytidine using LC-MS/MS to perform detailed pharmacokinetic studies. The drug of interest was extracted from plasma using Oasis MCX ion exchange solid-phase extraction 96-well plates. Chromatographic separation was achieved with an YMC J'sphere M80 C18 column and isocratic elution with a methanol-wat...

  13. Theory and Application of Mass Spectrometric Kinetic Method%质谱动力学方法原理及应用

    Institute of Scientific and Technical Information of China (English)

    李明; 李红梅; 熊行创; 江游; 黄泽建; 方向

    2012-01-01

    The mass spectrometric kinetic method based on the competitive dissociations of mass-selected cluster ions has been increasingly applied to thermochemical determination mainly due to its simplicity, speediness and sensitivity. Because the kinetic method employs tandem mass spectrometry, the compounds of interest need not be available in pure form. The kinetic method has been used to estimate gas-phase acidity and basicity and proton affinity, electron affinity, ionization energy, gas-phase basicities of multiply-charged biomole-cules, metal ion affinities, heterolytic bond dissociation energies, chiral recognition and quantification. In this paper the theory of kinetic method is introduced in detail and its applications are enumerated.%质谱动力学方法(Kinetic Method,简称KM法)是一种基于经质量选择的簇离子竞争解离反应速率的不同对热力学数据进行测定的方法,由于采用串联质谱技术,分析样品无需纯化,具有简便、快速、灵敏等优点.目前该方法已应用于气相酸碱度和质子亲合势的测定、电子亲和能的测定、电离能的测定、多电荷生物分子气相碱度的测定、金属离子与生物分子亲和力的测定、异裂离解能的测定、离子结构的检测及对手性化合物对映体过量的测定等.本工作在介绍质谱动力学方法原理的同时,列举了其应用实例,详细地对质谱动力学方法进行了综合述评.

  14. Characterization of Heavy Metal Contents in the Bulk Atmospheric Aerosols Simultaneously Collected at Three Islands in Okinawa, Japan by X-ray fluorescence spectrometric method (XRF)

    Science.gov (United States)

    Oshiro, Y.; ITOH, A.; Azechi, S.; Somada, Y.; Handa, D.; Miyagi, Y.; Arakaki, T.; Tanahara, A.

    2011-12-01

    We studied heavy metal contents of atmospheric aerosols using an X-ray fluorescence spectrometric method (XRF). The XRF method enables us to analyze heavy metal contents of bulk aerosols rapidly without any chemical pretreatments. We used an energy dispersive X-ray fluorescence spectrometer that is compact and portable. We prepared several different amounts of standard reference materials (NIES No.28) of Japanese National Institute of Environmental Studies on quartz filters for calibration curves. Then, we evaluated quantitative responses of XRF method by comparing with the metal contents determined by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after acid-digestion. Good linear relationships between X-ray intensity and amount of aerosol on filter were seen in the following 10 metals; Al, K, Ti, V, Fe, Ni, Rb, Ba, Pb and As. We then used XRF method to determine heavy metal contents in authentic atmospheric aerosols collected in Okinawa islands, Japan. Okinawa islands, consisting of many small islands, are situated east of Asian continent, and its location in Asian is well suited for studying long-range transport of air pollutants. Also, in Okinawa islands, maritime air mass prevails during summer, while Asian continental air mass dominates during fall, winter, and spring. The maritime air mass data can be seen as background clean air and can be compared with continental air mass which has been affected by anthropogenic activities such as industries and automobiles. Therefore, Okinawa region is suitable area for studying impacts of air pollutants from East Asia. We simultaneously collected bulk aerosol samples by using identical high-volume air samplers at 3 islands; Cape Hedo Atmospheric Aerosol Monitoring Station (CHAAMS, Okinawa island), Kume island (ca. 160 km south-west of CHAAMS), and Minami-Daitou island (ca. 320 km south-east of CHAAMS). We report and discuss spatial and temporal distribution of heavy metals

  15. The Composition of Titan's Lower Atmosphere and Simple Surface Volatiles as Measured by the Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer Experiment

    Science.gov (United States)

    Niemann, H. B.; Atreya, S. K.; Demick, J. E.; Gautier, D.; Haberman, J. A.; Harpold, D. N.; Kasprzak, W. T.; Lunine, J. I.; Owen, T. C.; Raulin, F.

    2010-01-01

    The Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer (GCMS) determined the composition of the Titan atmosphere from 140km altitude to the surface. After landing, it returned composition data of gases evaporated from the surface. Height profiles of molecular nitrogen (N2), methane (CH4) and molecular hydrogen (H2) were determined. Traces were detected on the surface of evaporating methane, ethane (C2H6), acetylene (C2H2), cyanogen (C2N2) and carbon dioxide (CO2). The methane data showed evidence that methane precipitation occurred recently. The methane mole fraction was (1.48+/-0.09) x 10(exp -2) in the lower stratosphere (139.8 km to 75.5 km) and (5.65+/-0.18) x 10(exp -2) near the surface (6.7 km to the surface). The molecular hydrogen mole fraction was (1.01+/-0.16) x 10(exp -3) in the atmosphere and (9.90+/-0.17) x 10(exp -4) on the surface. Isotope ratios were 167.7+/-0.6 for N-14/N-15 in molecular nitrogen, 91.1+/-1.4 for C-12/C-13 in methane and (1.35+/-0.30) x 10(exp -4) for D/H in molecular hydrogen. The mole fractions of Ar-36 and radiogenic Ar-40 are (2.1+/-0.8) x 10(exp -7) and (3.39 +/-0.12) x 10(exp -5) respectively. Ne-22 has been tentatively identified at a mole fraction of (2.8+/-2.1) x 10(exp -7) Krypton and xenon were below the detection threshold of 1 x 10(exp -8) mole fraction. Science data were not retrieved from the gas chromatograph subsystem as the abundance of the organic trace gases in the atmosphere and on the ground did not reach the detection threshold. Results previously published from the GCMS experiment are superseded by this publication.

  16. Liquid Chromatography-Electrospray Quadrupole Linear Ion Trap Mass Spectrometric Method for Quantitation of Domperidone in Chinese Healthy Volunteers

    Institute of Scientific and Technical Information of China (English)

    WU Yi; CHU Yang; ZHANG Yun-hui; WU Dan; GU Jing-kai

    2007-01-01

    A rapid, sensitive, and accurate method based on LC/MS/MS was developed and validated for the determination of domperidone in human plasma. Domperidone and internal standard, tramadol, were extracted from plasma with diethyl ether-dichloromethane(60: 40, volume ratio) and separated by reversed-phase HPLC with methanol-water-ammonia solution(80: 20: 0.2, volume ratio) as the mobile phase. Detection was carried out via multiple-reaction monitoring(MRM) on a Q-trapTM LC/MS/MS system(Q-trapTM). The assay result was linear over a concentration range of 0.1-30 ng/mL with a limit of quantitation (LOQ) of 0.1 ng/mL. The inter- and intra-day precision levels were within 7.52% and 12. 9%, respectively, whereas the accuracy was within a range of 87. 3%-114%. This method has been successfully applied to evaluate the pharmacokinetics of domperidone in Chinese healthy volunteers given an oral dose of 10 mg.

  17. Mass spectrometric method for the determination of the stable isotopic content of nitrous oxide by the technique of direct injection

    International Nuclear Information System (INIS)

    A method for the direct isotopic analysis of N2O has been developed for VG-Prism H dynamic dual inlet stable isotope mass spectrometer. Tests have shown extreme sensitivity to contamination by carbon dioxide with a dependence of 6.8 per mille per % CO2 for δ15N and 12.4 per mille per % CO2 for δ18O. Trace amounts of CO2 have proven difficult to eliminate, particularly for small sample sizes. In order to ensure accurate analyses an indicator of CO2 contamination must be monitored and corrections applied when necessary. We have found that ions with mass to charge ratios of 12 and 22 are excellent proxies for CO2 contamination. Empirical relationships between these indicator species and CO2 contamination are documented which allow for corrections to be applied to raw data. Additional corrections required due to the presence of isobaric molecules containing 17O are described. Issues of standardization are discussed and sample handling procedures described. Finally, these methods and corrections are applied to a suite of stratospheric air samples. (author)

  18. A robust and rapid liquid chromatography tandem mass spectrometric method for the quantitative analysis of 5-azacytidine.

    Science.gov (United States)

    Anders, Nicole M; Wanjiku, Teresia M; He, Ping; Azad, Nilofer S; Rudek, Michelle A

    2016-03-01

    The DNA methyltransferase inhibitor 5-azacytidine is being evaluated clinically as an oral formulation to treat various solid tumors. A sensitive, reliable method was developed to quantitate 5-azacytidine using LC-MS/MS to perform detailed pharmacokinetic studies. The drug of interest was extracted from plasma using Oasis MCX ion exchange solid-phase extraction 96-well plates. Chromatographic separation was achieved with a YMC J'sphere M80 C18 column and isocratic elution with a methanol-water-formic acid (15:85:0.1, v/v/v) mobile phase over a 7 min total analytical run time. An AB Sciex 5500 triple quadrupole mass spectrometer operated in positive electrospray ionization mode was used for the detection of 5-azacytidine. The assay range was 5-500 ng/mL and proved to be accurate (97.8-109.1%) and precise (CV ≤ 9.8%). Tetrahydrouridine was used to stabilize 5-azacytidine in blood/plasma samples. With the addition of tetrahydrouridine, long-term frozen plasma stability for 5-azacytidine at -70°C has been determined for at least 323 days. The method was applied for the measurement of total plasma concentrations of 5-azacytidine in a cancer patient receiving a 300 mg oral daily dose. PMID:26174363

  19. A robust and rapid liquid chromatography tandem mass spectrometric method for the quantitative analysis of 5-azacytidine

    Science.gov (United States)

    Anders, Nicole M.; Wanjiku, Teresia M.; He, Ping; Azad, Nilofer S.; Rudek, Michelle A.

    2015-01-01

    The DNA methyltransferase inhibitor 5-azacytidine is being evaluated clinically as an oral formulation to treat various solid tumors. A sensitive, reliable method was developed to quantitate 5-azacytidine using LC-MS/MS to perform detailed pharmacokinetic studies. The drug of interest was extracted from plasma using Oasis MCX ion exchange solid-phase extraction 96-well plates. Chromatographic separation was achieved with an YMC J'sphere M80 C18 column and isocratic elution with a methanol-water-formic acid (15:85:0.1, v/v/v) mobile phase over a 7 minute total analytical run time. An AB Sciex 5500 triple quadrupole mass spectrometer operated in positive electrospray ionization mode was used for the detection of 5-azacytidine. The assay range was 5 to 500 ng/mL and proved to be accurate (97.8-109.1%) and precise (%CV ≤9.8%). Tetrahydrouridine was used to stabilize 5-azacytidine in blood/plasma samples. With the addition of tetrahydrouridine, long-term frozen plasma stability for 5-azacytidine at -70°C has been determined for at least 323 days. The method was applied for the measurement of total plasma concentrations of 5-azacytidine in a cancer patient receiving a 300 mg oral daily dose. PMID:26174363

  20. Development of a cloud point extraction and preconcentration method for Cd and Ni prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Manzoori, Jamshid L. [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: manzoori@tabrizu.ac.ir; Karim-Nezhad, Ghasem [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2004-09-13

    In this work a new cloud point extraction (CPE) methodology was developed for the separation and preconcentration of cadmium and nickel. The analyte in the initial aqueous solution was complexed with dithizone and Triton X-114 was added as surfactant. After phase separation, based on the cloud point of the mixture, and dilution of the surfactant-rich phase with tetrahydrofuran (THF), the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions and preconcentration of only 10 ml of sample in the presence of 0.05% Triton X-114, the enhancement factors of 52 and 39 and the detection limits of 0.31 {mu}g l{sup -1} and 1.2 {mu}g l{sup -1} were obtained for cadmium and nickel respectively. The proposed method was applied satisfactorily to the determination of cadmium and nickel in water samples.

  1. In-house validation of a method for determination of silver nanoparticles in chicken meat based on asymmetric flow field-flow fractionation and inductively coupled plasma mass spectrometric detection

    DEFF Research Database (Denmark)

    Löschner, Katrin; Navratilova, Jana; Grombe, Ringo;

    2015-01-01

    spectrometric detection (AF4-ICP-MS) was applied for quantitative analysis of silver nanoparticles (AgNPs) in a chicken meat matrix following enzymatic sample preparation. For the first time an analytical validation of nanoparticle detection in a food matrix by AF4-ICP-MS has been carried out and the results......Nanomaterials are increasingly used in food production and packaging, and validated methods for detection of nanoparticles (NPs) in foodstuffs need to be developed both for regulatory purposes and product development. Asymmetric flow field-flow fractionation with inductively coupled plasma mass...

  2. Acquisition of a Gas Chromatograph/Mass Spectrometer System for Laboratory Study of Prebiotic Organic Geochemical Processes on the Early Earth, Mars, and Meteorites

    Science.gov (United States)

    McCollom, Thomas

    2004-01-01

    This was a major equipment grant that provided funds ($72K) for purchase of a benchtop gas chromatograph-mass spectrometer (GC-MS) for use in experimental studies of prebiotic organic compounds. An Agilent model 689015973 GC-MS was purchased and installed in the PI's lab in August of 2003. The instrument is now being used for a variety of research projects. The primary use of the instrument is to analyze and quantify organic products of laboratory experiments conducted by the PI. One example is shown, which shows organic products (predominantly n-alkanes) formed during Fischer-Tropsch-type abiotic synthesis under hydrothermal conditions. The analytical capabilities of the GC- MS allowed identification of the numerous organic products of this as well as other laboratory experiments. A key use of the instrument in this research is that the mass spectrometer capabilities allow use of isotopically labeled reactants to trace the progress of reactions and evaluate background contaminants. collaborative projects with other scientists involved in exobiology & astrobiology research (e.g., Mitch Schulte, NASA Ames; Katrina Edwards, Woods Hole Oceanographic Institution). For instance, an analysis of membrane lipids of an lithoautotrophic iron-oxidizing bacteria being grown on basalt as a source of metabolic energy, a project where the instrument is being used to evaluate possible biomarker compounds from these organisms is shown. These iron oxidizers are thought to be similar to those living within the ocean crust, and are being investigated as possible analog organisms to those on the early Earth or crust of Mars. The instrument has also been used by an outside investigator (graduate student Brandon Canfeld, Arizona State University) for identification and isotopic characterization of experimental products of abiotic organic synthesis experiments he is conducting with Dr. John Holloway. analysis of quality control samples for other NASA-funded projects. For instance, an

  3. Integration of Gas Chromatography Mass Spectrometry Methods for Differentiating Ricin Preparation Methods

    Energy Technology Data Exchange (ETDEWEB)

    Wunschel, David S.; Melville, Angela M.; Ehrhardt, Christopher J.; Colburn, Heather A.; Victry, Kristin D.; Antolick, Kathryn C.; Wahl, Jon H.; Wahl, Karen L.

    2012-05-17

    The investigation of crimes involving chemical or biological agents is infrequent, but presents unique analytical challenges. The protein toxin ricin is encountered more frequently than other agents and is found in the seeds of the castor plant Ricinus communis. Typically, the toxin is extracted from castor seeds utilizing a variety of different recipes that result in varying purity of the toxin. Moreover, these various purification steps can also leave or differentially remove a variety of exogenous and endogenous residual components with the toxin that may indicate the type and number of purification steps involved. We have applied three gas chromatographic - mass spectrometric (GC-MS) based analytical methods to measure the variation in seed carbohydrates and castor oil ricinoleic acid as well as the presence of solvents used for purification. These methods were applied to the same samples prepared using four previously identified toxin preparation methods starting from four varieties of castor seeds. The individual data sets for seed carbohydrate profiles, ricinoleic acid or acetone amount each provided information capable of differentiating different types of toxin preparations across seed types. However, the integration of the data sets using multivariate factor analysis provided a clear distinction of all samples based on the preparation method and independent of the seed source. In particular the abundance of mannose, arabinose, fucose, ricinoleic acid and acetone were shown to be important differentiating factors. These complementary tools provide a more confident determination of the method of toxin preparation.

  4. Gamma-spectrometric surveys in differentiated granites. I: a review of the method and of the geochemical behavior of K, Th and U

    International Nuclear Information System (INIS)

    This contribution is part of a research project on the Neo proterozoic Cunhaporanga Granitic Complex (CGC), cropping out in the Ponta Grossa Arch (Parana state, SE Brazil). An initial study used the gamma-spectrometric data of the Serra do Mar Sul Aero geophysical Project, performed during the 70's for CPRM. Later, terrestrial gamma-spectrometric surveys focused on the study of the differentiated Joaquim Murtinho Granite (JMG) in the NW corner of CGC, and the Serra do Carambei Granite, to the SW. In this paper, the results obtained for JMG are presented in two parts. The first deals with methodology and the presentation of several gamma-spectrometric 'color-scale' maps, indicating that results obtained in granites depend strongly on a climatic factor, given the mobility of K during weathering in subtropical climates with strong rainfalls, also favoring a greater mobility of U. Minerals that are U and Th hosts, documented in granites, are reviewed, together with the weathering processes that control the mobility of K, U and Th in soils. Strong K signals in granitic areas submitted to these climates document the presence of fresh rock and/or effects of hydrothermal alteration, while weak or nil signals are evidence of strong leaching of K during weathering. U and Th will be retained in the residual soils, in part leading to their selective enrichment, also coupled with soil migration to lower topographic levels by colluvial transport. The larger solubility of U (as uranyl ion) allows its liberation under oxidizing conditions, and its migration, limited by the possibility of absorption in newly formed mineral and organic soil phases. Th should be retained almost totally in resistant phases and, when liberated in solution, will mostly be fixed in organic and inorganic soil substances. (author)

  5. Analysis of Flavor Ingredients for Ruditapes Philippinarum by Headspace Solid-Phase Microextraction and Gas Chromatograph-Mass Spectrometer-Computer Method

    Directory of Open Access Journals (Sweden)

    Yun Ke

    2013-09-01

    Full Text Available To study the volatile flavor compound feature of Ruditapes philippinarum. The Ruditapes philippinarum flavor compounds were extracted with HS-SPME technology and identified combined with GC-MS. Twenty three kinds of flavor compounds were identified through the experience and the percentage composition of each flavor compound was further obtained. Conclusion: The research can provide a reference for the identification of aquatic product’s flavor feature with SPME and combined with GC-MS.

  6. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    OpenAIRE

    Hesham Salem

    2005-01-01

    Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate). The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed nati...

  7. Gamma-spectrometric Surveys in Differentiated Granites. I: a Review of the Method, and of the Geochemical Behavior of K, Th and U

    Directory of Open Access Journals (Sweden)

    Gilson Burigo Guimarães

    2009-01-01

    Full Text Available This contribution is part of a research project on the Neoproterozoic Cunhaporanga Granitic Complex (CGC, cropping out in thePonta Grossa Arch (Paraná state, SE Brazil. An initial study used the gamma-spectrometric data of the Serra do Mar Sul AerogeophysicalProject, performed during the 70’s for CPRM. Later, terrestrial gamma-spectrometric surveys focused on the study of the differentiatedJoaquim Murtinho Granite (JMG in the NW corner of CGC, and the Serra do Carambeí Granite, to the SW. In this paper,the results obtained for JMG are presented in two parts. The fi rst deals with methodology and the presentation of several gamma-spectrometric“color-scale” maps, indicating that results obtained in granites depend strongly on a climatic factor, given the mobility of Kduring weathering in subtropical climates with strong rainfalls, also favoring a greater mobility of U. Minerals that are U and Th hosts,documented in granites, are reviewed, together with the weathering processes that control the mobility of K, U and Th in soils. StrongK signals in granitic areas submitted to these climates document the presence of fresh rock and/or effects of hydrothermal alteration,while weak or nil signals are evidence of strong leaching of K during weathering. U and Th will be retained in the residual soils, in partleading to their selective enrichment, also coupled with soil migration to lower topographic levels by colluvial transport. The larger solubilityof U (as uranyl ion allows its liberation under oxidizing conditions, and its migration, limited by the possibility of absorptionin newly formed mineral and organic soil phases. Th should be retained almost totally in resistant phases and, when liberated in solution,will mostly be fi xed in organic and inorganic soil substances.

  8. Gamma-spectrometric definition of natural radionuclide content in soil

    International Nuclear Information System (INIS)

    The method of gamma-spectrometric definition if natural radionuclide content in soil is proposed that takes into account the loosened contribution of natural background constituent in measured spectra. The radioactivity of some territories of Uzbekistan is investigated by the present method. (author)

  9. Determination of Palladium in Resin by Lead Fire Assaying-Flame Atomic Absorption Spectrometric Method%铅试金富集-火焰原子吸收光谱法测定树脂中钯

    Institute of Scientific and Technical Information of China (English)

    王芳; 陈小兰; 林海山; 李小玲; 肖红新

    2013-01-01

    通过铅试金富集树脂中的钯并用银作钯灰吹保护,得到的银钯合粒用王水溶解,在5%的盐酸介质中,采用原子吸收光谱法测定钯,该法测钯的相对标准偏差RSD为0.53%,加标回收率在99.04%~100.10%之间。%Palladium in resin was enriched by lead assaying, using silver as a protective agent to produce silver-palladium alloy, and then the alloy was dissolved in aqua regia. Air acetylene flame atomic absorption spectrometric method was used to determinate palladium in 5%hydrochloric acid solution. The relative standard deviation (RSD) in determination of palladium is 0.53%and the recovery rate is between 99.04%~100.10%.

  10. Inventory of metal complexes circulating in plant fluids: a reliable method based on HPLC coupled with dual elemental and high-resolution molecular mass spectrometric detection.

    Science.gov (United States)

    Flis, Paulina; Ouerdane, Laurent; Grillet, Louis; Curie, Catherine; Mari, Stéphane; Lobinski, Ryszard

    2016-08-01

    Description of metal species in plant fluids such as xylem, phloem or related saps remains a complex challenge usually addressed either by liquid chromatography-mass spectrometry, X-ray analysis or computational prediction. To date, none of these techniques has achieved a complete and true picture of metal-containing species in plant fluids, especially for the least concentrated complexes. Here, we present a generic analytical methodology for a large-scale (> 10 metals, > 50 metal complexes) detection, identification and semiquantitative determination of metal complexes in the xylem and embryo sac liquid of the green pea, Pisum sativum. The procedure is based on direct injection using hydrophilic interaction chromatography with dual detection by elemental (inductively coupled plasma mass spectrometry) and molecular (high-resolution electrospray mass spectrometry) mass spectrometric detection. Numerous and novel complexes of iron(II), iron(III), copper(II), zinc, manganese, cobalt(II), cobalt(III), magnesium, calcium, nickel and molybdenum(IV) with several ligands including nicotianamine, citrate, malate, histidine, glutamine, aspartic acid, asparagine, phenylalanine and others are observed in pea fluids and discussed. This methodology provides a large inventory of various types of metal complexes, which is a significant asset for future biochemical and genetic studies into metal transport/homeostasis. PMID:27111838

  11. Analysis Method for Pesticides Residues by GC/MS in Lebanese Apple

    International Nuclear Information System (INIS)

    The apple's crop can be affected by many pests during the growing season, which requires careful monitoring. Both apple fruit and apple tree need to be treated by pesticides in order to protect them from pests. Such treatment often leads to the accumulation of stable pesticides inside the fruit. The local market provides a large variety of pesticides allowing farmers to use more than one active substance in order to protect their crop, often without proper advice. Monitoring pesticides on apples and other agricultural crops is the best way to protect consumers health from the hazards of pesticides residues. The development of new, rapid and effective method to analyze the multi pesticides residues at trace levels in apple samples is essential. This work describes the extraction procedure and the analytical method developed to detect the pesticide residues using the gas-chromatographic-mass spectrometric approach (GC-MS). The developed method was successfully applied to analyze apple samples collected from different Lebanese markets for a one year period in order to monitor the presence of pesticides and their stability in apple fruits during storage. (author)

  12. Mass spectrometric isotope dilution analysis of small calcium concentrations in minerals

    International Nuclear Information System (INIS)

    A mass spectrometric isotope dilution analysis for the determination of small calcium contents is developed. The different steps (decomposition of the mineral including isotope dilution technique, calcium separation and mass spectrometric measurement) of the analytical procedure are described. For a 42Ca spike the optimum spike addition is calculated. The dependence of the analysis error on the mass spectrometric measurements is discussed. Using a chromatographic method with a strong acidic ion exchanger calcium can be completely separated from potassium. The calcium content in the range of 0.15-0.004% of two feldspars and of one lepidolite is determined with external relative standard deviations of 0.9-5.1%. (orig.)

  13. Development of a hydrophilic interaction liquid chromatography-tandem mass spectrometric method for the determination of kinsenoside, an antihyperlipidemic candidate, in rat plasma and its application to pharmacokinetic studies.

    Science.gov (United States)

    Rehman, Shaheed Ur; Kim, In Sook; Choi, Min Sun; Luo, Zengwei; Yao, Guangming; Xue, Yongbo; Zhang, Yonghui; Yoo, Hye Hyun

    2016-02-20

    Kinsenoside is a major bioactive constituent isolated from Anoectochilus formosanus and is investigated as an antihyperlipidemic candidate. In this study, a rapid, sensitive, and reliable bioanalytical method was developed for the determination of kinsenoside in rat plasma using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). The plasma sample was pretreated with 1% acetic acid, followed by protein precipitation with acetonitrile:methanol (70:30). Chromatographic separation was performed on a HILIC silica column (2.1mm×100mm, 3μm). The mobile phases consisted of 0.1% acetic acid in distilled water (solvent A) and 0.1% acetic acid in acetonitrile (solvent B). A gradient program was used at a flow rate of 0.2mL/min. For mass spectrometric detection, the multiple reaction monitoring mode was used; the MRM transitions were m/z 265.2→m/z 102.9 for kinsenoside and m/z 163.3→m/z 132.1 for the internal standard (IS) nicotine in the positive ionization mode. A calibration curve was constructed in the range of 2-500ng/mL. The intra- and interday precision and accuracy were within 5%. The HILIC-MS/MS method was specific, accurate, and reproducible and was successfully applied in a pharmacokinetic study of kinsenoside in rats. PMID:26686829

  14. Development and validation of a sensitive liquid chromatographic-tandem mass spectrometric method for the simultaneous analysis of granisetron and 7-hydroxy granisetron in human plasma and urine samples: application in a clinical pharmacokinetic study in pregnant subject.

    Science.gov (United States)

    Zhao, Yang; Chen, Hui-Jun; Caritis, Steve; Venkataramanan, Raman

    2016-02-01

    A liquid chromatography-tandem mass spectrometric method for the quantification of granisetron and its major metabolite, 7-hydroxy granisetron in human plasma and urine samples was developed and validated. Respective stable isotopically labeled granisetron and 7-hydroxy granisetron were used as internal standards (IS). Chromatography was performed using an Xselect HSS T3 analytical column with a mobile phase of 20% acetonitrile in water (containing 0.2 mM ammonium formate and 0.14% formic acid, pH 4) delivered in an isocratic mode. Tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring was used for quantification. The standard curves were linear in the concentration ranges of 0.5-100 ng/mL for granisetron and 0.1-100 ng/mL for 7-hydroxy granisetron in human plasma samples, and 2-2000 ng/mL for granisetron and 2-1000 ng/mL for 7-hydroxy granisetron in human urine samples, respectively. The accuracies were >85% and the precision as determined by the coefficient of variations was <10%. No significant matrix effects were observed for granisetron or 7-hydroxy granisetron in either plasma or urine samples. Granisetron was stable under various storage and experimental conditions. This validated method was successfully applied to a pharmacokinetic study after intravenous administration of 1 mg granisetron to a pregnant subject. PMID:26053159

  15. Identification of irradiated pasteurized egg products: a combined method to use in routine control

    International Nuclear Information System (INIS)

    Pasteurized egg products (whole egg, egg yolk and egg white) were tested for irradiation treatment in the German food control laboratories in Oldenburg/Niedersachsen and Kassel/Hessen as well as in the food irradiation laboratory of the German federal health office. Gas chromatographic/mass spectrometric measurements on the fat components of egg-products showed clearly whether the product had been irradiated or not. While in unirradiated samples no traces of special hydrocarbons (according to the fatty acid composition of egg) and no traces of the irradiation-specific compound 2-Dodecyl-cyclobutanone were found, irradiated control samples as well as products of two belgian suppliers contained these substances. Additionally, regarding the rather high time consumption of gas chromatography, electron spin resonance (ESR)-measurements were carried out on the packaging material of egg products. Irradiated packaging material (cellulose) could be easily detected by the appearance of a signal pair in the ESR spectrum (cellulose radical). ESR measurements are very fast and easy to perform so that this method can be used for screening. Microbiological investigations showed remarkably reduced total numbers of microorganisms for some irradiated samples, but the microbiological status is influenced by other factors like storage-time and -temperature, so that microbiological tests can not be used successfully for screening on irradiation treatment

  16. Measurement of methyl tert-butyl ether and tert-butyl alcohol in human blood by purge-and-trap gas chromatography-mass spectrometry using an isotope-dilution method.

    Science.gov (United States)

    Bonin, M A; Ashley, D L; Cardinali, F L; McCraw, J M; Wooten, J V

    1995-01-01

    We developed an isotope-dilution method for measuring methyl tert-butyl ether (MTBE) and tert-butyl alcohol (TBA) in whole human blood using a purge-and-trap gas chromatographic-mass spectrometric method. The labeled analogues for MTBE and TBA were [2H12]methyl tert-butyl ether and [2H9]-tert-butyl alcohol, respectively. Volatiles were removed from the blood by direct helium purging of the liquid; were trapped on a Tenax trap; and were desorbed, cryofocused, and chromatographed on a DB-624 capillary column that was connected directly to the ion source of a mass spectrometer. Detection was by mass analysis using a double-focusing magnetic-sector mass spectrometer operating in the full-scan mode at the medium mass resolution of 3000. For the isotope-dilution method, the minimum detection limits in blood (5-10 mL) are 0.01 microgram/L for MTBE and 0.06 microgram/L for TBA. The isotope-dilution method proved to be a big improvement in recovery, reproducibility, and sensitivity over our previous analytical method, which used the labeled ketone, [4-2H3]-2-butanone, as the internal standard for both MTBE and TBA. The isotope-dilution method has sufficient sensitivity for monitoring blood levels of MTBE and TBA in populations exposed to oxygenated fuels containing MTBE. PMID:7564298

  17. Electrospray Ionization Mass Spectrometric Analysis of Highly Reactive Glycosyl Halides

    Directory of Open Access Journals (Sweden)

    Lajos Kovács

    2012-07-01

    Full Text Available Highly reactive glycosyl chlorides and bromides have been analysed by a routine mass spectrometric method using electrospray ionization and lithium salt adduct-forming agents in anhydrous acetonitrile solution, providing salient lithiated molecular ions [M+Li]+, [2M+Li]+ etc. The role of other adduct-forming salts has also been evaluated. The lithium salt method is useful for accurate mass determination of these highly sensitive compounds.

  18. Development, validation and application of an ultra high performance liquid chromatographic-tandem mass spectrometric method for the simultaneous detection and quantification of five different classes of veterinary antibiotics in swine manure.

    Science.gov (United States)

    Van den Meersche, Tina; Van Pamel, Els; Van Poucke, Christof; Herman, Lieve; Heyndrickx, Marc; Rasschaert, Geertrui; Daeseleire, Els

    2016-01-15

    In this study, a fast, simple and selective ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the simultaneous detection and quantification of colistin, sulfadiazine, trimethoprim, doxycycline, oxytetracycline and ceftiofur and for the detection of tylosin A in swine manure was developed and validated. First, a simple extraction procedure with acetonitrile and 6% trichloroacetic acid was carried out. Second, the supernatant was evaporated and the pellet was reconstituted in 1 ml of water/acetonitrile (80/20) and 0.1% formic acid. Extracts were filtered and analyzed by UHPLC-MS/MS on a Kinetex C18 column using gradient elution. The method developed was validated according to the criteria of Commission Decision 2002/657/EC. Recovery percentages varied between 94% and 106%, repeatability percentages were within the range of 1.7-9.2% and the intralaboratory reproducibility varied between 2.8% and 9.3% for all compounds, except for tylosin A for which more variation was observed resulting in a higher measurement uncertainty. The limit of detection and limit of quantification varied between 1.1 and 20.2 and between 3.5 and 67.3 μg/kg, respectively. This method was used to determine the presence and concentration of the seven antibiotic residues in swine manure sampled from ten different manure pits on farms where the selected antibiotics were used. A link was found between the antibiotics used and detected, except for ceftiofur which is injected at low doses and degraded readily in swine manure and was therefore not recovered in any of the samples. To the best of our knowledge, this is the first method available for the simultaneous extraction and quantification of colistin with other antibiotic classes. Additionally, colistin was never extracted from swine manure before. Another innovative aspect of this method is the simultaneous detection and quantification of five different classes of antibiotic residues in swine manure

  19. Ultra-sensitive Mass Spectrometric and Other Advanced Methods Applied to Biological Samples. Second interlaboratory comparison study for the analysis of 239Pu in synthetic urine at the μBq (∼100 aCi) level by mass spectrometry

    International Nuclear Information System (INIS)

    As a follow up to the initial 1998 intercomparison study, a second study was initiated in 2001 as part of the ongoing evaluation of the capabilities of various ultra-sensitive methods to analyze 239Pu in urine samples. The initial study was sponsored by the Department of Energy, Office of International Health Programs to evaluate and validate new technologies that may supersede the existing fission tract analysis (FTA) method for the analysis of 239Pu in urine at the μBq/l level. The ultra-sensitive techniques evaluated in the second study included accelerator mass spectrometry (AMS) by LLNL, thermal ionization mass spectrometry (TIMS) by LANL and FTA by the University of Utah. Only the results for the mass spectrometric methods will be presented. For the second study, the testing levels were approximately 4, 9, 29 and 56 μBq of 239Pu per liter of synthetic urine. Each test sample also contained 240Pu at a 240Pu/239Pu atom ratio of ∼0.15 and natural uranium at a concentration of 50 μBq/ml. From the results of the two studies, it can be inferred that the best performance at the μBq level is more laboratory specific than method specific. The second study demonstrated that LANL-TIMS and LLNL-AMS had essentially the same quantification level for both isotopes. Study results for bias and precision and acceptable performance compared to ANSI N13.30 and ANSI N42.22 have been compiled. (author)

  20. A Validated High-Performance Liquid Chromatography-Tandem Mass Spectrometric (Lc-Ms/Ms Method for Simultaneous Determination of R(+-Ketorolac and S(−-Ketorolac in Human Plasma and Its Application to a Bioequivalence Study

    Directory of Open Access Journals (Sweden)

    Sabyasachi Patri

    2011-01-01

    Full Text Available We report a selective, accurate, and reproducible liquid chromatography-tandem mass spectrometric (LC-MS/MS method that employs solid phase extraction for quantification of ketorolac enantiomers in human plasma. Resolution of R(+-ketorolac and S(−-ketorolac was achieved using a Chiral-AGP column and a mobile phase of ammonium formate buffer (10 mM, pH 4.70±0.05:acetonitrile (85 : 15, v/v and 70 : 30, v/v in a gradient time program. S(+-etodolac was used as the internal standard (IS. Quantification was achieved using a positive electrospray ionization (ESI+ interface under multiple reaction monitoring (MRM condition. The method was validated over the concentration range of 9.36–1198.69 ng/ml for R(+-ketorolac and 6.07–776.74 ng/ml for S(−-ketorolac. Matrix effect was found negligible and the method showed good performances in terms of accuracy (89.6–102.7% and precision (1.7–6.7% for both enantiomers. Extraction recoveries of R(+-ketorolac, S(−-ketorolac, and S(+-etodolac were 82.04, 70.94, and 93.90%, respectively. Results of all stability exercises in human plasma were within acceptable limits. The method was successfully applied to a single dose cross over bioequivalence study in healthy human male volunteers. Incurred Sample Reanalysis (ISR was performed by randomly selecting 10% of total subject samples of the study using Statistical Analysis Software (SAS. Values of 91.1% for R (+-ketorolac and 83.5% for S(−-ketorolac indicated good acceptance for ISR.

  1. Qualification and application of a liquid chromatography-tandem mass spectrometric method for the determination of human Aβ1-40 and Aβ1-42 peptides in transgenic mouse plasma using micro-elution solid phase extraction.

    Science.gov (United States)

    Shin, Young G; Hamm, Lee; Murakami, Stanley; Buirst, Kenji; Buonarati, Michael H; Cox, April; Regal, Kelly; Hunt, Kevin W; Scearce-Levie, Kimberly; Watts, Ryan J; Liu, Xingrong

    2014-05-01

    A liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method was developed and applied for the determination of human Aβ1-40 and Aβ1-42 peptides in transgenic mouse plasma to support preclinical pharmacodynamics studies. The method consisted of micro-elution solid phase extraction for sample preparation and LC-MS/MS analysis in the negative ion mode using electrospray ionization for analysis. (15)N53-Aβ1-40 and (15)N55-Aβ1-42 peptides were used as internal standards. A quadratic regression (weighted 1/concentrations), with an equation y = ax(2) + bx + c, was used to fit calibration curves over the concentration range of 0.500-100 ng/mL for both Aβ1-40 and Aβ1-42 peptides. For quality control samples at 6.00, 40.0 and 80.0 ng/mL from the qualification experiment, the within-run accuracy ranged from -2.69 to 0.583 % with precision values ≤8.23 % for Aβ1-40. Within-run accuracy ranged from -4.83 to 10.1 % with precision values ≤8.87 % for Aβ1-42. Samples from a pharmacodynamics study using Tg2576 transgenic mice were analyzed by this qualified LC-MS/MS method and concentrations were compared to those generated by ELISA. The two methods were shown to be comparable for Aβ1-40 quantification of samples from the Tg2576 amyloid precursor protein transgenic mouse model, but varied slightly for Aβ1-42. PMID:23888333

  2. Impact of the grinding process on the quantification of ethyl glucuronide in hair using a validated UPLC-ESI-MS-MS method.

    Science.gov (United States)

    Kummer, Natalie; Wille, Sarah M R; Di Fazio, Vincent; Ramírez Fernández, Maria Del Mar; Yegles, Michel; Lambert, Willy E E; Samyn, Nele

    2015-01-01

    The Society of Hair Testing (SoHT) has provided cutoffs for the quantification of ethyl glucuronide (EtG) in hair to indicate occasional or chronic/excessive alcohol consumption. Although several sensitive methods have been reported, past proficiency test results show a lack of reproducibility. An ultra-performance liquid chromatographic mass spectrometric method (LLOQ of 10 pg EtG/mg hair) has been validated according to the international guidelines, including the successful participation in five proficiency tests. This method was subsequently used to evaluate the impact of different grinding conditions (cut, weakly or extensively pulverized hair samples) on the final measured EtG concentration. Hair from alcohol consumers (n = 2) and commercially available quality control samples (QCs) (n = 2) was used. For the QCs, extensive pulverization led to a significantly higher amount of measured EtG. In the hair samples obtained from volunteers, cut or weakly pulverized hair resulted in EtG concentrations below the LLOQ, while the mean concentrations of 14 and 40 pg EtG/mg hair were determined after extensive pulverization. Differences in sample preparation could partially explain inter-laboratory variability. As the differences in results can lead to a different interpretation even when applying the SoHT cutoffs, it is of interest to standardize sample preparation techniques in the field of EtG hair testing. PMID:25274495

  3. Validation of a liquid chromatography-triple quadrupole mass spectrometric method for the determination of 5-nitro-5'-hydroxy-indirubin-3'-oxime (AGM-130) in human plasma and its application to microdose clinical trial.

    Science.gov (United States)

    Park, Min-Ho; Lee, Yun Young; Cho, Kyung Hee; La, Sookie; Lee, Hee Joo; Yim, Dong-Seok; Ban, Sooho; Park, Moon-Young; Kim, Yong-Chul; Kim, Yoon-Gyoon; Shin, Young G

    2016-03-01

    A liquid chromatography-triple quadrupole mass spectrometric (LC-MS/MS) method was developed and validated for the determination of 5-nitro-5'-hydroxy-indirubin-3'-oxime (AGM-130) in human plasma to support a microdose clinical trial. The method consisted of a liquid-liquid extraction for sample preparation and LC-MS/MS analysis in the positive ion mode using TurboIonSpray(TM) for analysis. d3 -AGM-130 was used as the internal standard. A linear regression (weighted 1/concentration) was used to fit calibration curves over the concentration range of 10-2000 pg/mL for AGM-130. There were no endogenous interference components in the blank human plasma tested. The accuracy at the lower limit of quantitation was 96.6% with a precision (coefficient of variation, CV) of 4.4%. For quality control samples at 30, 160 and 1600 pg/mL, the between run CV was ≤5.0 %. Between-run accuracy ranged from 98.1 to 101.0%. AGM-130 was stable in 50% acetonitrile for 168 h at 4°C and 6 h at room temperature. AGM-130 was also stable in human plasma at room temperature for 6 h and through three freeze-thaw cycles. The variability of selected samples for the incurred sample reanalysis was ≤12.7% when compared with the original sample concentrations. This validated LC-MS/MS method for determination of AGM-130 was used to support a phase 0 microdose clinical trial. PMID:26139072

  4. A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue.

    Science.gov (United States)

    Yue, Hongfei; Jansen, Susan A; Strauss, Kenneth I; Borenstein, Michael R; Barbe, Mary F; Rossi, Luella J; Murphy, Elise

    2007-02-19

    A sensitive, specific, and robust liquid chromatography/mass spectrometric (LC/MS) method was developed and validated that allows simultaneous analysis of arachidonic acid (AA) and its cyclooxygenase, cytochrome P450, and lipoxygenase pathway metabolites prostaglandins (PGs), dihydroxyeicosatrienoic acids (DiHETrEs), hydroxyeicosatetraenoic acids (HETEs) and epoxyeicosatrienoic acids (EETs), including PGF(2alpha), PGE(2), PGD(2), PGJ(2), 14,15-DiHETrE, 11,12-DiHETrE, 8,9-DiHETrE, 5,6-DiHETrE, 20-HETE, 15-HETE, 12-HETE, 9-HETE, 8-HETE, 5-HETE, 14,15-EET, 11,12-EET, 8,9-EET, and 5,6-EET in rat brain tissues. Deuterium labeled PGF(2alpha)-d(4), PGD(2)-d(4), 15(S)-HETE-d(8), 14,15-EET-d(8), 11,12-EET-d(8), 8,9-EET-d(8), and AA-d(8) were used as internal standards. Solid phase extraction was used for sample preparation. A gradient LC/MS method using a C18 column and electrospray ionization source under negative ion mode was optimized for the best sensitivity and separation within 35 min. The method validation, including LC/MS instrument qualification, specificity, calibration model, accuracy, precision (without brain matrix and with brain matrix), and extraction efficiency were performed. The linear ranges of the calibration curves were 2-1000 pg for PGs, DiHETrEs, HETEs, and EETs, 10-2400 pg for PGE(2) and PGD(2), and 20-2000 ng for AA, respectively. PMID:17125954

  5. Characterization of nuclear fuels by ICP mass-spectrometric techniques

    International Nuclear Information System (INIS)

    Isotopic analyses of radioactive materials such as irradiated nuclear fuel are of major importance for the optimization of the nuclear fuel cycle and for safeguard aspects. Among the mass-spectrometric techniques available, inductively coupled plasma mass spectrometry (ICP-MS) and thermal ionization mass spectrometry are the most frequently applied methods for nuclear applications. Because of the low detection limits, the ability to analyze the isotopic composition of the elements and the applicability of the techniques for measuring stable as well as radioactive nuclides with similar sensitivity, both mass-spectrometric techniques are an excellent amendment to classical radioactivity counting methods. The paper describes selected applications of multicollector ICP-MS in combination with chromatographic separation techniques and laser ablation for the isotopic analysis of irradiated nuclear fuels. The advantages and limitations of the selected analytical technique for the characterization of such a heterogeneous sample matrix are discussed. (orig.)

  6. High sensitivity liquid chromatography tandem mass spectrometric methods for the analysis of dioctyl sulfosuccinate in different stages of an oil spill response monitoring effort.

    Science.gov (United States)

    Ramirez, Cesar E; Batchu, Sudha Rani; Gardinali, Piero R

    2013-05-01

    After the incident on the Deepwater Horizon platform, around 1.8 million gallons of dispersants were used in the field as part of the response cleanup efforts. This study describes an online solid phase extraction-liquid chromatography (LC)-tandem mass spectrometry (MS/MS) method and a direct-injection LC-MS/MS method for the analysis of dioctyl sulfosuccinate (DOSS; a component in Corexit® EC9500A) in seawater at trace levels, with method detection limits (MDLs) of 7.0 and 440 ng/L and run times of 7 and 17 min, respectively. Stability and preservation studies demonstrated that samples at 4.7 μg/L could be preserved for up to 150 days without loss of analyte when stored with 33 % acetonitrile in glass containers. Data acquisition was performed by heated electrospray ionization (ESI) MS/MS operating in negative mode. Methods were validated in terms of percent recovery in fortified blank and matrix samples and to evaluate carryover. A simple modification of the direct-injection method allowed quantitation of 2-butoxyethanol, a dispersant component specific to the Corexit® EC9527A formulation. This method was used to simultaneously quantify DOSS and 2-butoxyethanol in two Corexit® formulations and extracts from an MC-252 source oil standard. MDLs in crude oil were 0.723 and 4.46 mg/kg, respectively, with recoveries of (92 ± 9)% for DOSS and (104 ± 8)% for 2-butoxyethanol. Detection of both indicators was achieved in a single chromatographic run by ESI-MS/MS operating sequentially in positive and negative mode. Corexit® EC9500A and Corexit® EC9527A were found to contain (21 ± 2)% and (22 ± 5)% w/w DOSS and 0 and (37 ± 2)% w/w 2-butoxyethanol, respectively. PMID:23471369

  7. Confirmation of the correct application of the gamma spectrometric method carried out in the Cuban Center for Radiation Protection and Hygiene

    International Nuclear Information System (INIS)

    One of the technical requirements of the standard ISO/IEC 17025:2006 is that the laboratories that use standard methods shall confirm that they can properly operate these before introducing the tests or calibrations. Among the testing activities that execute the Environmental Radiological Surveillance Laboratory of the Cuban Center for Radiation Protection and Hygiene, is the determination of gamma radionuclides by gamma spectrometry with HPGe detectors. This test has been accredited by the Cuban Accreditation Body, according to the standard ISO/IEC 17025:2005. Fulfilling the requirements of this standard, regarding the selection of methods, the laboratory uses internationally standard method for its gamma spectrometry determinations. For this reason it was necessary to confirm the correct application of the selected method before incorporating it as scientific-technical service that the institution offers. With this purpose the method confirmation using certified reference materials of different matrixes and for the different geometries used in the laboratory were carried out. The obtained results of this study were processed statistically to check the precision and trueness of the same ones. In this sense, the laboratory participates periodically in interlaboratory comparison programs that include the radionuclides analysis by gamma spectrometry, as another form of accuracy confirmation of the results that the laboratory reports. In this paper the design of the realized intralaboratory study, as well as the results of it are presented. From the obtained results in the realized study, as well as from the interlaboratory comparison programs, it is possible to conclude that the method used in the laboratory is executed appropriately and it is under control. (author)

  8. A rapid gas chromatographic injection-port derivatization method for the tandem mass spectrometric determination of patulin and 5-hydroxymethylfurfural in fruit juices.

    Science.gov (United States)

    Marsol-Vall, Alexis; Balcells, Mercè; Eras, Jordi; Canela-Garayoa, Ramon

    2016-07-01

    A novel method consisting of injection-port derivatization coupled to gas chromatography-tandem mass spectrometry is described. The method allows the rapid assessment of 5-hydroxymethylfurfural (HMF) and patulin content in apple and pear derivatives. The chromatographic separation of the compounds was achieved in a short chromatographic run (12.2min) suitable for routine controls of these compounds in the fruit juice industry. The optimal conditions for the injection-port derivatization were at 270°C, 0.5min purge-off, and a 1:2 sample:derivatization reagent ratio (v/v). These conditions represent an important saving in terms of derivatization reagent consumption and sample preparation time. Quality parameters were assessed for the target compounds, giving LOD of 0.7 and 1.6μg/kg and LOQ of 2 and 5μg/kg for patulin and HMF, respectively. These values are below the maximum patulin concentration in food products intended for infants and young children. Repeatability (%RSD n=5) was below 12% for both compounds. In addition, the method linearity ranged between 25 and 1000μg/kg and between 5 and 192μg/kg for HMF and patulin, respectively. Finally, the method was applied to study HMF and patulin content in various fruit juice samples. PMID:27240947

  9. A liquid chromatography tandem mass spectrometric method on in vitro nerve agents poisoning characterization and reactivator efficacy evaluation by determination of specific peptide adducts in acetylcholinesterase.

    Science.gov (United States)

    Yan, Long; Chen, Jia; Xu, Bin; Guo, Lei; Xie, Yan; Tang, Jijun; Xie, Jianwei

    2016-06-10

    The terroristic availability of highly toxic nerve agents (NAs) highlights the necessity for a deep understanding of their toxicities and effective medical treatments. A liquid chromatography tandem mass spectrometry (LC-MS/MS) method for a characterization of the NAs poisoning and an evaluation on the efficacy of reactivators in in vitro was developed for the first time. After exposure to sarin or VX and pepsin digestion, the specific peptides of acetylcholinesterase (AChE) in a purified status, i.e. undecapeptide "GESAGAASVGM" in free, unaged, or aged status was identified and quantified. A key termination procedure is focused to make the reaction system "frozen" and precisely "capture" the poisoning, aging and spontaneous reactivation status of AChE, and the abundance of such specific peptides can thus be simultaneously measured. In our established method, as low as 0.72% and 0.84% inhibition level of AChE induced by 0.5nM sarin and VX can be detected from the measurement of peptide adducts, which benefits a confirmation of NAs exposure, especially at extremely low levels. Comparing with conventional colorimetric Ellman assays, our method provides not only enzyme activity and inhibition rate, but also the precise poisoning status of NAs exposed AChE. Based on the full information provided by this method, the efficacy of reactivators, such as HI-6, obidoxime and pralidoxime, in the typical treatment of NAs poisoned AChE in in vitro was further evaluated. Our results showed that this method is a promising tool for the characterization of NAs poisoning and the evaluation of reactivator efficacy. PMID:27179675

  10. A mass spectrometric method for rapidly assaying the chiral selectivities of the copper(I) complexes of C2-symmetric ligands.

    Science.gov (United States)

    Davis, Mark C; Gronert, Scott

    2015-11-01

    A gas-phase method for rapidly assaying the enantioselectivity of metal-centered catalysts is presented. It relies on gas-phase equilibrium measurements in a quadrupole ion trap mass spectrometer. A group of well-established C2-symmetric bis-oxazoline copper(I) complexes was used to identify chiral probe reagents that are capable of profiling the quality of the asymmetric environment provided by the metal complex. The chiral probes were then applied to a wide variety of copper(I) bis-di-imine complexes. Complexes based on a BINAM backbone exhibited selectivities that were comparable to the bis-oxazolines. Taking advantage of the mass selectivity capabilities of the ion trap mass spectrometer, the method was also applied to an un-purified mix of copper(I) complexes derived from a combinatorial synthesis of bis-di-imine ligands. This approach holds promise as a rapid screening tool for potential chiral catalysts. PMID:26505773

  11. Experimental determination of the chemical changes in the electron density on indium nuclei by the γ-spectrometric ΔIγ/Iγ method

    International Nuclear Information System (INIS)

    The γ-spectrometry method for determination of the relative change ΔλEC/λEC in the partial probability λEC for the 114mIn decay branch by the electron capture (EC), when the nucleus is in different chemical environments, was developed. The method is based on an experimental determination of the relative change ΔIγ/Iγ in the intensity of the γ-radiation which is emitted by the excited daughter 114Cd nuclei after EC. The 114mIn decay by EC in indium metal, In2O3 and InAs was compared. The largest ΔIγ/Iγ=(2.5±0.8).10-4 has been found for InAs relatively to In2O3. The chemical changes in the electron density on the indium nucleus corresponding to the measured ΔIγ/Iγ values have been determined

  12. Comparison of various liquid chromatographic methods involving UV and atmospheric pressure chemical ionization mass spectrometric detection for the efficient trace analysis of phenylurea herbicides in various types of water samples.

    Science.gov (United States)

    van der Heeft, E; Dijkman, E; Baumann, R A; Hogendoorn, E A

    2000-05-19

    The performance of mass spectrometric (MS) detection and UV detection in combination with reversed-phase liquid chromatography without and with the use of coupled column RPLC (LC-LC) has been compared for the trace analysis of phenylurea herbicides in environmental waters. The selected samples of this comparative study originated from an inter-laboratory study. For both detection modes, a 50 mm x 4.6 mm I.D. column and a 100 mm x 4.6 mm I.D. column packed with 3 microm C18 were used as the first (C-1) and second (C-2) column, respectively. Atmospheric pressure chemical ionization mass spectrometry was performed on a magnetic sector instrument. The LC-LC-MS analysis was carried out on-line by means of direct large volume (11.7 ml) injection (LVI). The performance of both on-line (LVI, 4 ml of sample) and off-line LC-LC-UV (244 nm) analysis was investigated. The latter procedure consisted of a solid-phase extraction (SPE) of 250 ml of water sample on a 500 mg C18 cartridge. The comparative study showed that LC-LC-MS is more selective then LC-LC-UV and, in most cases, more sensitive. The LVI-LC-LC-MS approach combines direct quantification and confirmation of most of the analytes down to a level of 0.01 microg/l in water samples in less then 30 min. As regards LC-LC-UV, the off-line method appeared to be a more viable approach in comparison with the on-line procedure. This method allows the screening of phenylurea's in various types of water samples down to a level of at least 0.05 microg/l. On-line analysis with LVI provided marginal sensitivity (limits of detection of about 0.1 microg/l) and selectivity was sometimes less in case of surface water samples. Both the on-line LVI-LC-LC-MS method and the LC-LC-UV method using off-line SPE were validated by analysing a series of real-life reference samples. These samples were part of an inter-laboratory test and contained residues of herbicides ranging from 0.02 to 0.8 microg/l. Beside good correlation between the methods

  13. Determination of divalent iron content in igneous rocks of ultrabasic, basic and intermediate compositions by a wavelength-dispersive X-ray fluorescence spectrometric method

    International Nuclear Information System (INIS)

    This paper proposes the quantitative wavelength-dispersive X-ray fluorescence (XRF) technique of divalent iron content determination in igneous rocks and reports specifics of this technique in terms of classifying rocks into ultrabasic, basic, intermediate and acid ones. Unlike the widely used technique of titration, the proposed XRF technique does not require a labor-consuming procedure for sample preparation. In the fields of FeKβ5 line, and FeKβ′ and FeKβ″ satellites relative intensities of XRF emission spectrum lines are dependent on the valence state of iron in minerals. The ratio FeKβ5/FeKβ1,3 is preferred as the analytical parameter. The XRF method allows divalent iron content (expressed as FeO oxide) over 1.5% to be measured in igneous rocks of ultrabasic and basic compositions by the common calibration equation with the error below 10 rel. %, that is comparable with the error of titrimetric analysis. The samples of igneous rocks of intermediate composition and granodiorites should be analyzed using calibration equations obtained with certified reference materials corresponding in composition to the study samples. For the samples of alkaline rocks the errors of FeO content determination might be in excess of 50 rel. %. - Highlights: • The wavelength-dispersive X-ray fluorescence method allows the determination of divalent iron contents. • Separate calibrations should be used for different types of igneous rocks. • Errors of X-ray fluorescence method and titrimetric analysis are comparable

  14. Enantioseparation and determination of isofenphos-methyl enantiomers in wheat, corn, peanut and soil with Supercritical fluid chromatography/tandem mass spectrometric method.

    Science.gov (United States)

    Chen, Xixi; Dong, Fengshou; Xu, Jun; Liu, Xingang; Chen, Zenglong; Liu, Na; Zheng, Yongquan

    2016-03-15

    Supercritical fluid chromatography/tandem mass spectrometry (SFC-MS/MS) is an effective tool in separation science which uses the nontoxic CO2 fluid for better control of analyte retention. Also the technology of a postcolumn additive to complement MS/MS ensure the high-selectivity determination. In this paper, a green and sensitive analytical method was developed for the enantioselective separation and determination of isofenphos-methyl enantiomers in foodstuff and soil by SFC-MS/MS. The enantioseparation was performed within 3.50min using Chiralpak IA-3 column with CO2/isopropanol (90:10, v/v) as the mobile phase at 2.2mL/min flow rate. The postcolumn compensation technology provided with 0.1% formic acid/methanol greatly improved the ionization efficiency of mass spectrometry. Column temperature, auto back pressure regulator pressure, and flow rate of compensation solvent were optimized to 30°C, 2200psi, and 0.1mL/min, respectively. The QuEChERs method was adopted in this study, which mean recoveries of isofenphos-methyl enantiomers ranged from 75.7% to 111.4%, with relative standard deviations less than 11.3% at three concentration levels in all matrices. The limits of detection for both enantiomers varied from 0.02μg/kg to 0.15μg/kg, while the limit of quantification did not exceed 0.50μg/kg. The proposed method was then successfully applied to analyze authentic samples, confirming that it was a versatile strategy for the analysis of isofenphos-methyl enantiomers in food and environmental matrices. PMID:26894851

  15. Determination of total lead in lipstick: development and validation of a microwave-assisted digestion, inductively coupled plasma-mass spectrometric method.

    Science.gov (United States)

    Hepp, Nancy M; Mindak, William R; Cheng, John

    2009-01-01

    Recent reports describing the presence of lead (Pb) in lipsticks have suggested that, under ordinary use, the potential amount of Pb exposure is harmful. To permit independent assessment of the Pb contamination, a method for determining total Pb in lipstick using microwave-assisted digestion and analysis employing inductively coupled plasma-mass spectrometry (ICP-MS) was developed and validated. Since lipsticks may contain fats, oils, pigments, dyes, and minerals, several reference materials (RM) were analyzed, including coal, wear metals in oil, organic Pb in oil, milk powder, and estuarine sediment. With the exception of the RM with mineral content (estuarine sediment), complete recovery of Pb from the RMs was obtained by simple nitric acid (HNO(3)) digestion. Complete recovery of Pb from estuarine sediment was achieved only when hydrofluoric acid (HF) was added to the digestion mix, followed by treatment with excess boric acid (H(3)BO(3)) to neutralize the HF and to dissolve insoluble fluorides. Commercial lipsticks were tested for total Pb by the validated method. The detection limit was estimated to be 0.04 microg Pb/g. The average value obtained for the lipsticks was 1.07 microg/g. Undigested material was present in some lipstick digests when only HNO(3) was used, and generally lower Pb values were obtained. All of the Pb levels found by the U.S. Food and Drug Administration (FDA) were within the range the agency would expect to find in lipsticks formulated with permitted color additives and other ingredients prepared under good manufacturing practice (GMP) conditions. This method will be useful for the FDA and industry in helping to ensure the safety of cosmetic products. PMID:19691936

  16. Development of an isotope labeling ultra-high performance liquid chromatography mass spectrometric method for quantification of acylglycines in human urine

    International Nuclear Information System (INIS)

    Graphical abstract: - Abstract: Acylglycines play a crucial regulatory and detoxification role in the accumulation of the corresponding acyl CoA esters and are an important class of metabolites in the diagnoses of inborn errors of metabolism. Sensitive quantification of a large number of acylglycines not only improves diagnosis but also enables the discovery of potential new biomarkers of diseases. We report an ultra-high performance liquid chromatography tandem mass spectrometry (UPLC–MS) method for quantifying acylglycines in human urine with high sensitivity. This method is based on the use of a newly developed isotope labeling reagent, p-dimethylaminophenacyl (DmPA) bromide, to label acylglycines to improve detection sensitivity. Eighteen acylglycines, namely acetylglycine, propionylglycine, isobutyrylglycine, butyrylglycine, 4-hydroxyphenylacetylglycine, 2-furoylglycine, tiglylglycine, 2-methybutyrylglycine, 3-methylcrotonylglycine, isovalerylglycine, valerylglycine, hexanoylglycine, phenylacetylglycine, phenylpropionylglycine, glutarylglycine, heptanoylglycine, octanoylglycine and suberylglycine, were measured. This method uses calibration standards prepared in surrogate matrix (un-derivatized urine) and stable-isotope labeled analytes as the internal standards. The analysis was carried out in the positive ion detection mode using multiple reaction monitoring (MRM) survey scans. The calibration curves were validated over the range of 1.0–500 nM. The method achieved a lower limit of quantitation (LLOQ) of 1–5 nM for all analytes, as measured by the standard derivations associated with calibration curves and confirmed in surrogate matrix; the signal-to-noise ratio at LLOQ ranged from 12.50 to 156.70. Both accuracy (% RE or relative error) and precision (% CV) were <15%. Matrix effects were minimized using the surrogate matrix. All eighteen analytes were stable in urine for at least 5 h at room temperature, autosampler (4 °C) for 24 h, 7 weeks at −20

  17. Gas chromatographic–mass spectrometric validated method for the determination of Bisphenol A in public-supply water: An investigation in Campo Grande, MS, Brazil

    Directory of Open Access Journals (Sweden)

    Émerson Montagner

    2013-01-01

    Full Text Available A new validated method is described for determining bisphenol A (BPA in surface and public-supply water samples. Recovery rates of 91% to 113%, with coefficients of variation below 8.9%, were obtained within the limit of detection (2.4 ng L–1. Concentrations of 13 to 113 ng L–1 were found in tap water. An analysis of BPA stability in solid-phase extraction cartridges revealed that the analyte can be stored in such containers for at least 90 days. An evaluation of BPA leached from polyvinyl chloride (PVC piping showed that BPA can contaminate water distribution systems.

  18. A new preconcentration and separation method for flame atomic absorption spectrometric determinations of some trace metal ions on a diaion HP-20 column

    International Nuclear Information System (INIS)

    A preconcentration/separation method for determination of Cr(3), Cd(2), Bi(3) and Co(2) has been proposed. The analytes were adsorbed on a column filled Diaion HP-20 resin as metal-8-hydroxiquinoline complexes and desorbed from the column by using 10 ml of 1M HNO3 in acetone. The influences of some analytical parameters such as pH, amounts of oxine, type of eluent etc on the recoveries of chromium, cadmium, bismuth and cobalt were discussed. Effects of the various alkaline salts on the recoveries of the investigated ions were also examined. The method was applied for the determination of Cr(3), Cd(2), Bi(3), and Co(2) contents of table salt samples, some chemical grade alkaline salts produced in Turkey and a stream sediment standard reference material sample (GBW 07309) with satisfactory results (recoveries > 95%, relative standard deviations < 9%). The limit of detection for analyte ions (3s, N=20) was between 23-305 ng/g

  19. Development and validation of a supercritical fluid chromatography method for the direct determination of enantiomeric purity of provitamin B5 in cosmetic formulations with mass spectrometric detection.

    Science.gov (United States)

    Khater, Syame; West, Caroline

    2015-01-01

    A rapid and efficient chiral supercritical fluid chromatography (SFC) method has been developed for the quantitative determination of panthenol enantiomers in cosmetic formulations (cream, lotion, wipe, and exfoliant). Indeed, the pharmacological effect only depends on the D form (Dexpanthenol) thus accurate measurement of its enantiomeric purity in formulated cosmetic products is of interest. The samples were prepared with liquid-liquid extraction followed by solid-phase extraction on Adsorbex amino cartridges. After testing several enantioselective columns in an attempt at reversing the elution order to have the minor enantiomer eluted first, the best separation of enantiomers and internal standard (N-acetyl-L-alanine) was achieved on a 3 μm-amylose-type immobilized polysaccharide chiral stationary phase (Chiralpak IA) in less than 6 min with a simple mobile phase comprising carbon dioxide and 11% methanol pumped at 2.3 mL/min, 25°C and 150 bar backpressure. Supercritical fluid chromatography coupled to both an optical diode-array detector and a user-friendly single-quadrupole mass spectrometer (Waters QDa) equipped with electrospray ionization source has been used. The on-line coupling ensures the technique to be more informative and improves detection sensitivity, as underivatized panthenol has a poor UV absorption. The limit of quantification (LOQ) achieved with single-ion recording was 0.5 μg/mL. The method was validated in terms of linearity, precision and accuracy and satisfactory results were obtained. PMID:25459930

  20. Validation of a liquid chromatography-electrospray ionization tandem mass spectrometric method to determine six polyether ionophores in raw, UHT, pasteurized and powdered milk.

    Science.gov (United States)

    Pereira, Mararlene Ulberg; Spisso, Bernardete Ferraz; Jacob, Silvana do Couto; Monteiro, Mychelle Alves; Ferreira, Rosana Gomes; Carlos, Betânia de Souza; da Nóbrega, Armi Wanderley

    2016-04-01

    This study aimed to validate a method developed for the determination of six antibiotics from the polyether ionophore class (lasalocid, maduramicin, monensin, narasin, salinomycin and semduramicin) at residue levels in raw, UHT, pasteurized and powdered milk using QuEChERS extraction and high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The validation was conducted under an in-house laboratory protocol that is primarily based on 2002/657/EC Decision, but takes in account the variability of matrix sources. Overall recoveries between 93% and 113% with relative standard deviations up to 16% were obtained under intermediate precision conditions. CCα calculated values did not exceed 20% the Maximum Residue Limit for monensin and 25% the Maximum Levels for all other substances. The method showed to be simple, fast and suitable for verifying the compliance of raw and processed milk samples regarding the limits recommended by Codex Alimentarius and those adopted in European Community for polyether ionophores. PMID:26593474

  1. Fluorinated carbon tag derivatization combined with fluorous solid-phase extraction: a new method for the highly sensitive and selective mass spectrometric analysis of glycans.

    Science.gov (United States)

    Li, Lulu; Jiao, Jing; Cai, Yan; Zhang, Ying; Lu, Haojie

    2015-01-01

    The sensitive and specific detection of glycans via mass spectrometry (MS) remains a significant challenge due to their low abundance in complex biological mixtures, inherent lack of hydrophobicity, and suppression by other, more abundant biological molecules (proteins/peptides) or contaminants. A new strategy for the sensitive and selective MS analysis of glycans based on fluorous chemistry is reported. Glycan reducing ends were derivatized with a hydrophobic fluorinated carbon tag, increasing glycan ionization efficiency during MS by more than an order of magnitude. More importantly, the fluorinated carbon tag enabled efficient fluorous solid-phase extraction (FSPE) to specifically enrich the glycans from contaminated solutions and protein mixtures. Finally, we successfully analyzed the N-glycome in human serum using this new method. PMID:25884104

  2. Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Bhavin N. [Chemistry Department, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380 009, Gujarat (India); Analytical Laboratory, BA Research India Ltd., Bodakdev, Ahmedabad 380 054, Gujarat (India); Sharma, Naveen [Analytical Laboratory, BA Research India Ltd., Bodakdev, Ahmedabad 380 054, Gujarat (India); Sanyal, Mallika [Chemistry Department, St. Xaviers' College, Navrangpura, Ahmedabad 380 009, Gujarat (India); Shrivastav, Pranav S. [Chemistry Department, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380 009, Gujarat (India)], E-mail: pranav_shrivastav@yahoo.com

    2008-11-23

    A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the simultaneous determination of donepezil (D) and its pharmacologically active metabolite, 6-O-desmethyl donepezil (6-ODD) in human plasma is developed using galantamine as internal standard (IS). The analytes and IS were extracted from 500 {mu}L aliquots of human plasma via solid-phase extraction (SPE) on Waters Oasis HLB cartridges. Chromatographic separation was achieved in a run time of 6.0 min on a Waters Novapak C18 (150 mm x 3.9 mm, 4 {mu}m) column under isocratic conditions. Detection of analytes and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The protonated precursor to product ion transitions monitored for D, 6-ODD and IS were at m/z 380.1 {yields} 91.2, 366.3 {yields} 91.3 and 288.2 {yields} 213.2, respectively. The method was fully validated for its selectivity, interference check, sensitivity, linearity, precision and accuracy, recovery, matrix effect, ion suppression/enhancement, cross-specificity, stability and dilution integrity. A linear dynamic range of 0.10-50.0 ng mL{sup -1} for D and 0.02-10.0 ng mL{sup -1} for 6-ODD was evaluated with mean correlation coefficient (r) of 0.9975 and 0.9985, respectively. The intra-batch and inter-batch precision (%CV, coefficient of variation) across five quality control levels was less than 7.5% for both the analytes. The method was successfully applied to a bioequivalence study of 10 mg donepezil tablet formulation in 24 healthy Indian male subjects under fasting condition.

  3. Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method

    International Nuclear Information System (INIS)

    A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the simultaneous determination of donepezil (D) and its pharmacologically active metabolite, 6-O-desmethyl donepezil (6-ODD) in human plasma is developed using galantamine as internal standard (IS). The analytes and IS were extracted from 500 μL aliquots of human plasma via solid-phase extraction (SPE) on Waters Oasis HLB cartridges. Chromatographic separation was achieved in a run time of 6.0 min on a Waters Novapak C18 (150 mm x 3.9 mm, 4 μm) column under isocratic conditions. Detection of analytes and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The protonated precursor to product ion transitions monitored for D, 6-ODD and IS were at m/z 380.1 → 91.2, 366.3 → 91.3 and 288.2 → 213.2, respectively. The method was fully validated for its selectivity, interference check, sensitivity, linearity, precision and accuracy, recovery, matrix effect, ion suppression/enhancement, cross-specificity, stability and dilution integrity. A linear dynamic range of 0.10-50.0 ng mL-1 for D and 0.02-10.0 ng mL-1 for 6-ODD was evaluated with mean correlation coefficient (r) of 0.9975 and 0.9985, respectively. The intra-batch and inter-batch precision (%CV, coefficient of variation) across five quality control levels was less than 7.5% for both the analytes. The method was successfully applied to a bioequivalence study of 10 mg donepezil tablet formulation in 24 healthy Indian male subjects under fasting condition

  4. A solid liquid extraction and preconcentration method for the atomic absorption spectrometric determination of trace cobalt in various alloys and biological samples

    International Nuclear Information System (INIS)

    Cobalt is quantitatively retained as cobalt-2-nitroso-4-sulfonic acid (nitros-S)-tetradecyldimethylbenzylammonium (TDBA+) ion-pair complex on microcrystalline naphthalene in the pH range 6.2-9.0 from a large volume of its aqueous solution of various complex samples. After filtration, the solid mass consisting of cobalt complex and naphthalene is dissolved in 5 ml of dimethylformamide (DMF) and the metal is determined by flame atomic absorption spectrometry (FAAS). Cobalt complex can alternatively be quantitatively adsorbed on tetradecyldimethylbenzylammonium chloride-naphthalene adsorbent packed in a column and determined similarly. The calibration curve is linear over the concentration range 0.2-11.5 μg of cobalt in 5 ml of the final DMF solution. In this case, 0.2 μg of cobalt may be concentrated in a column from 250 ml of aqueous sample where its concentration is as low as 0.8 ng/ml. Eight replicate determinations of 3.0 μg of cobalt in the final DMF solution give a mean absorbance of 0.045 with a relative standard deviation of 1.8%. The sensitivity for 1% absorption is 59 ng/ml. The interference of a large number of anions and cations on the determination of cobalt has been studied and the optimum conditions developed utilized for its trace determination in various alloys and biological samples. The method may also be used for the determination of cobalt in some environmental samples

  5. Determination of divalent iron content in igneous rocks of ultrabasic, basic and intermediate compositions by a wavelength-dispersive X-ray fluorescence spectrometric method

    Science.gov (United States)

    Chubarov, Victor M.; Finkelshtein, Alexandr L.

    2015-05-01

    This paper proposes the quantitative wavelength-dispersive X-ray fluorescence (XRF) technique of divalent iron content determination in igneous rocks and reports specifics of this technique in terms of classifying rocks into ultrabasic, basic, intermediate and acid ones. Unlike the widely used technique of titration, the proposed XRF technique does not require a labor-consuming procedure for sample preparation. In the fields of FeKβ5 line, and FeKβ‧ and FeKβ″ satellites relative intensities of XRF emission spectrum lines are dependent on the valence state of iron in minerals. The ratio FeKβ5/FeKβ1,3 is preferred as the analytical parameter. The XRF method allows divalent iron content (expressed as FeO oxide) over 1.5% to be measured in igneous rocks of ultrabasic and basic compositions by the common calibration equation with the error below 10 rel. %, that is comparable with the error of titrimetric analysis. The samples of igneous rocks of intermediate composition and granodiorites should be analyzed using calibration equations obtained with certified reference materials corresponding in composition to the study samples. For the samples of alkaline rocks the errors of FeO content determination might be in excess of 50 rel. %.

  6. Determination of polybrominated diphenyl ethers in house dust using standard addition method and gas chromatography with electron capture and mass spectrometric detection.

    Science.gov (United States)

    Król, Sylwia; Zabiegała, Bożena; Namieśnik, Jacek

    2012-08-01

    Monitoring of the environmental fate of polybrominated diphenyl ethers (PBDEs) involves determination of their concentration in air, airborne particles and settled dust. This requires the implementation of appropriate analytical tools like measuring instruments, reference materials and analytical procedures. In this study an analytical procedure was developed for determining PBDEs in samples with a complex matrix composition. The efficiencies of three different extraction techniques - Soxhlet extraction (SE), Accelerated Solvent Extraction (ASE) and Ultrasound Assisted Extraction (UAE) - were compared. The study investigated the possibility of using the standard addition method for estimating PBDEs levels. The GC-μECD system was successfully applied as an alternative to low resolution mass spectrometry (LRMS) for determining BDE-209 in dust samples. The developed analytical procedure was then used to analyze dust samples, collected from houses and computer suites in the Tri-city area (Gdansk, Gdynia and Sopot), in order to detect and quantify the presence of polybrominated diphenyl ethers (PBDEs) in the indoor environment. Concentrations of studied congeners (from triBDE to heptaBDE), obtained by chromatographic analysis of dust samples extracts, performed applying two measurement systems (GC-EIMS and GC-μECD) ranged between 331 and 3102 ng g(-1) for house dust and between

  7. Mass spectrometric thermodynamic studies of oxide systems and materials

    Science.gov (United States)

    Stolyarova, V. L.

    2016-01-01

    Progress in methods of synthesis of advanced materials as well as utilization of such materials at high temperatures requires information on the vaporization processes and thermodynamic properties of oxide systems. The optimal experimental method for these purposes is high-temperature mass spectrometry. This review summarizes and classifies experimental results obtained in mass spectrometric studies of the high-temperature thermodynamic properties of oxide systems and materials carried out in the last two decades. Published data on the vaporization processes and thermodynamic properties of oxide materials for high-temperature technologies are discussed from the standpoint of acid-base concept and model approaches including statistical thermodynamic methods. The bibliography includes 248 references.

  8. 分光光度计法快速检测果汁中嗜热耐酸菌%A Rapid Spectrometric Method for Detecting Alicyclobacillus acidoterrestris in Fruit Juice

    Institute of Scientific and Technical Information of China (English)

    叶建芳; 李文俊; 赵文超; 莫小晶; 贾彩凤

    2011-01-01

    酸土脂环酸芽孢杆菌(Alicyclobacillus acidoterrestris)是果汁污染的主要嗜酸耐热菌。它可以将香草酸或者香兰素转化为愈创木酚,后者在过氧化物酶的作用下产生红褐色产物,从而可以快速检测该菌。根据这个原理,设计实验探究该颜色反应的最优培养条件以及实际体系中检测该菌的可行性。结果表明:在静止培养情况下,在BAM培养基中添加100μg/kg的香草酸最有利于愈创木酚的产生;不同浓度的嗜热耐酸菌芽孢液在上述条件下培养,随着浓度的降低产生高浓度愈创木酚时间依次延迟,最低浓度为3个/mL的芽孢%In the presence of AlicyclobaciUus acidoterrestris, vanillic acid and vanillin can be converted into guaiacol, which can be further converted into a reddish-brown product by peroxidase. Based on this color reaction, a method was developed to spectrometrically detect the presence of Alicyclobacillus acidoterrestris in real systems. In static culture, BAM medium with the addition of 100 μg/kg vanillic acid was the most favorable for gualacol formation. The peak value of guaiacol concentration was delayed along with the decrease of bacteria concentration. A visible color was formed in medium and its OD470 could reach up to 1.0 or even more after 21 hours of culture at the initial spore density of 3 spores/mL. And the same result also was obtained in an apple juice system. Thus, this method can allow rapid, simple and sensitive detection ofAlicyclobacillus acidoterrestris in fruit juice.

  9. The accuracy of X-ray fluorescence spectrometric determination of Rb and Sr contents in rock sample

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering method in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide element contents at an accuracy level +- 1 %

  10. The hydrolysis of aluminium, a mass spectrometric study

    OpenAIRE

    Sarpola, A.

    2007-01-01

    Abstract This thesis is focused on the hydrolysis of aluminium, the polymerisation of the hydrolysis products, and how these can be monitored by mass spectrometric methods. The main aim of this research is to figure out how the aqueous speciation of aluminium changes as a function of pH (3.2–10), concentration (1–100 mM), reaction time (1s–14d), and counter anion (Cl-, SO42-, HCOO-). The method used was electrospray mass spectrometry. The results showed more variable speciation than those ...

  11. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    Robert De Levie

    2009-09-01

    The spectrometric analysis of a mixture of two chemically and spectroscopically similar compounds is illustrated for the simultaneous spectrometric determination of caffeine and theobromine, the primary stimulants in coffee and tea, based on their ultraviolet absorbances. Their analysis indicates that such measurements may need an unexpectedly high precision to yield accurate answers, because of an artifact of inverse cancellation, in which a small noise or drift signal is misinterpreted in terms of a concentration difference. The computed sum of the concentrations is not affected.

  12. Photometric and emission-spectrometric determination of boron in steels

    International Nuclear Information System (INIS)

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.)

  13. Photometric and emission-spectrometric determination of boron in steels

    Energy Technology Data Exchange (ETDEWEB)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated.

  14. Gamma spectrometric assessment of nuclear fuel

    Science.gov (United States)

    Krištof, Edvard; Pregl, Gvido

    1990-12-01

    A description is given of a gamma spectrometric technique which has been developed with the aim of determining the amount of a certain radioactive fission product taking into consideration local variations of the linear attenuation coefficient of gamma rays. Also, an experiment using a fuel element of the TRIGA Mark II reactor in Ljubljana is presented.

  15. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    Directory of Open Access Journals (Sweden)

    Hesham Salem

    2005-01-01

    Full Text Available Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate. The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed native fluorescence at 450 nm when excitation was at 290 nm. The calibration graph was rectilinear from 0.3-1.4 μg mL-1 (method I. Cobalt sulphate was used for precipitation of the ion associates formed from the reaction with the cited drugs. The formation and solubility of the solid complexes at the optimum conditions of pH and ionic strength values have been studied. The method depends on direct determination of the ions in the precipitate or indirect determination of the ions in the filtrate by atomic absorption spectroscopy. The optimum conditions for precipitation were carefully studied. Rectilinear calibration graphs were obtained in the range of 3-30 μg mL-1 for each of the investigated drugs. The molar ratios of the formed chelats were determined by Job's method and their association constants were also calculated (method II. Ammonium vanadate was used for the spectrophotometric determination of the selected fluoroquinolones by oxidation in sulphuric acid medium resulting in the development of a greenish blue colour measured at 766 nm which was attributed to the vanadium (IV produced by reduction of vanadium (V by the selected drugs. The optimum conditions for heating time, reagent concentration and sulphuric acid concentration were carefully studied. The accuracy and precision of the proposed method was confirmed by estimating five or six replicates within Beer's law limits were obtained in the range 10-40 μg mL-1 for each of the investigated drugs

  16. Mass-spectrometric monitoring of the stress reaction during anesthesia

    Science.gov (United States)

    Elizarov, A. Yu.; Levshankov, A. I.; Faizov, I. I.; Shchegolev, A. V.

    2013-10-01

    Clinical testing data for a mass-spectrometric method of estimating the patient's stress reaction to an injury done during anesthesia are presented. The essence of the method is monitoring the respiratory coefficient, which is defined as ratio N of the expiratory mass concentration of CO2 to the inspiratory mass concentration of O2 at each breathing cycle. For on-line monitoring of N, an electron ionization mass spectrometer connected to the breathing circuit of an inhalational anesthesia machine is used. Estimates of the anesthesia adequacy obtained with this method are compared with those obtained with the method that analyzes induced acoustic encephalographic potentials. It is shown that the method suggested is more sensitive to the level of the patient's stress reaction during anesthesia than the induced potential method.

  17. X-ray spectrometric determination of thorium in bone and other biological materials

    International Nuclear Information System (INIS)

    An x-ray spectrometric method has been developed for the determination of thorium in bone and other biological materials. The limit of detection at the 95% confidence level is 20 ng. This corresponds to a concentration of 2 ppb in a 10-g sample of bone ash

  18. The analysis of comet mass spectrometric data

    Science.gov (United States)

    Balm, S. P.; Hare, J. P.; Kroto, H. W.

    1991-04-01

    The mass spectra from the Giotto PICCA experiment have been studied using computer simulations based on tabulated mass spectrometric data. It is shown that random mixtures of organic compounds give rise to mass spectra with peaks at about 45, 60, 75, and 90 amu; i.e., separated by about 15 amu. In particular it is shown that the products of Urey-Miller type experiments give mass spectra which can match the observed Giotto data closely. The analysis indicates that the material consists mainly of C/H/O/N (i.e., it is organic), but that the assignment to any well defined organic material is less certain. It is not clear that mass spectrometric studies of complex mixtures have the prospect of yielding this type of information without some form of preseparation.

  19. Commercial Applications of X Ray Spectrometric Techniques

    International Nuclear Information System (INIS)

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z ≥ 10, with a few instruments capable of detecting also elements with Z ≥ 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg’s law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  20. Targeted quantitative mass spectrometric immunoassay for human protein variants

    Directory of Open Access Journals (Sweden)

    Nedelkov Dobrin

    2011-04-01

    Full Text Available Abstract Background Post-translational modifications and genetic variations give rise to protein variants that significantly increase the complexity of the human proteome. Modified proteins also play an important role in biological processes. While sandwich immunoassays are routinely used to determine protein concentrations, they are oblivious to protein variants that may serve as biomarkers with better sensitivity and specificity than their wild-type proteins. Mass spectrometry, coupled to immunoaffinity separations, can provide an efficient mean for simultaneous detection and quantification of protein variants. Results Presented here is a mass spectrometric immunoassay method for targeted quantitative proteomics analysis of protein modifications. Cystatin C, a cysteine proteinase inhibitor and a potential marker for several pathological processes, was used as a target analyte. An internal reference standard was incorporated into the assay, serving as a normalization point for cystatin C quantification. The precision, linearity, and recovery characteristics of the assay were established. The new assay was also benchmarked against existing cystatin C ELISA. In application, the assay was utilized to determine the individual concentration of several cystatin C variants across a cohort of samples, demonstrating the ability to fully quantify individual forms of post-translationally modified proteins. Conclusions The mass spectrometric immunoassays can find use in quantifying specific protein modifications, either as a part of a specific protein biomarker discovery/rediscovery effort to delineate the role of these variants in the onset of the disease, progression, and response to therapy, or in a more systematic study to delineate and understand human protein diversity.

  1. Reference instruments based on spectrometric measurement with Lucas Cells

    International Nuclear Information System (INIS)

    The Bundesamt fuer Strahlenschutz (Berlin, Germany) and the Paul Scherrer Institute (Villigen, Switzerland) both operate accredited calibration laboratories for radon gas activity concentration. Both the institutions use Lucas Cells as detector in their reference instrumentation due to the low dependence of this detector type on variations in environmental conditions. As a further measure to improve the quality of the reference activity concentration, a spectrometric method of data evaluation has been applied. The electric pulses from the photomultiplier tube coupled to the Lucas Cells are subjected to a pulse height analysis. The stored pulse height spectra are analysed retrospectively to compensate for fluctuations in the electric parameters of the instrumentation during a measurement. The reference instrumentation of both the laboratories is described with the respective spectrum evaluation procedures. The methods of obtaining traceability to the primary calibration laboratories of Germany and Switzerland and data of performance tests are presented. (authors)

  2. Characterization of tetanus toxin, neat and in culture supernatant, by electrospray mass spectrometry

    NARCIS (Netherlands)

    Baar, B.L.M. van; Hulst, A.G.; Roberts, B.; Wils, E.R.J.

    2002-01-01

    A method was developed for the liquid chromatographic-mass spectrometric (LC-MS) identification of extremely neurotoxic toxins. The method combines sample treatment in a safety containment and analysis of detoxified material in a common laboratory facility. The method was applied to the characteriza

  3. Mass spectrometric analysis of integral membrane proteins: application to complete mapping of bacteriorhodopsins and rhodopsin.

    OpenAIRE

    Ball, L. E.; Oatis, J. E.; Dharmasiri, K.; Busman, M.; Wang, J.; Cowden, L. B.; Galijatovic, A.; N. Chen; Crouch, R K; Knapp, D R

    1998-01-01

    Integral membrane proteins have not been readily amenable to the general methods developed for mass spectrometric (or internal Edman degradation) analysis of soluble proteins. We present here a sample preparation method and high performance liquid chromatography (HPLC) separation system which permits online HPLC-electrospray ionization mass spectrometry (ESI-MS) and -tandem mass spectrometry (MS/MS) analysis of cyanogen bromide cleavage fragments of integral membrane proteins. This method has...

  4. Identification of organic iodocompounds in the PUREX process with the help of methods for chromatographic separation and spectrometric detection as well as characterization of their behavior during extraction. Final report

    International Nuclear Information System (INIS)

    In the system HNO3 KI, Dodecan and TBP the radiolytic reactive behaviour of the described compounds during the dissolution of nuclear fuel elements was simulated. External γ-irradiation gave the best informations. As a consequence of radiolyticly induced reactions several volatile and non-volatile iodoorganic compounds like iodoalkanes, iodonitroalkanes and iodonitroalkylphosphates are formed. They were separated by gaschromatography (GC) and high performance liquid chromatography (HPLC). For HPLC a special photolytic/electrochemical detector with comparable sensitivity like the electroncapture detector in the GC-field was developed. With the help of the two described chromatographic techniques the different iodoorganic compounds could be separated singularily or in groups of isomers. The separation of all compounds demands two-dimensional chromatographies including the capillary-SFC, which was not available for this project. Most of the iodoorganic compounds could be identified by comparison of the retention times of well known compounds. In the other cases, the compounds were studied mass-spectrometrically. Unfortunately all available ionisation techniques (EI; CI; FAB) were too hard for the labile C-I-bond. Therefore an identification of these compounds was not possible. In any case, instructive fingerprint spectra are available enabling relationships between the generation of the iodoorganic compounds and the reaction conditions during their formation. (orig.)

  5. Mass spectrometric examinations of Hungarian triassic dolomites

    International Nuclear Information System (INIS)

    A limited number of mass spectrometric investigations (viz.:57) of representative rock types were applied both in the research work of geology and the mining for the industry of building materials of Hungary. Tabulated results covering all rock types and all stratigraphic levels of the Hungarian Triassic are given. Sr, Mn, Ti and Cr trace elements had the highest occurrence and Zn, Y or Pb, Ba, V or Cu, depending on the genetical type of the rock studied, has relatively higher concentrations as well. The results of the examinations of Hungarian Triassic dolomites were discussed according to genetical types, all represented by a small level of trace elements. (Sz.J.)

  6. Accuracy of X-ray fluorescence spectrometric determination of Rb and Sr concentrations in rock samples

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering for matrix correction in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide concentrations at a relative accuracy level of 1%. The empirical method applies to rock samples showing differences in mass absorption up to a factor of two. The accuracy of the method has been tested by analysis of 57 samples analysed for Rb and Sr by mass spectrometric isotope dilution. In addition a few of the U.S. Geological Survey reference rock powders, showing significantly different mass absorption, were analysed for Rb and Sr. It is demonstrated that the mica effect, if significant, is smaller than 1% relative. There is no advantage in the use of the LiF(220) analysing crystal as a substitute for the LiF(200). The method appears to be insensitive to the pellet thickness. (author)

  7. Spectrometric differentiation of yeast strains using minimum volume increase and minimum direction change clustering criteria

    OpenAIRE

    Fachada, Nuno; Figueiredo, Mário A. T.; Lopes, Vitor V.; Martins, Rui C.; Rosa, Agostinho

    2014-01-01

    This paper proposes new clustering criteria for distinguishing Saccharomyces cerevisiae (yeast) strains using their spectrometric signature. These criteria are introduced in an agglomerative hierarchical clustering context, and consist of: (a) minimizing the total volume of clusters, as given by their respective convex hulls; and, (b) minimizing the global variance in cluster directionality. The method is deterministic and produces dendrograms, which are important features for microbiologists...

  8. Quantification of salsolinol enantiomers by stable isotope dilution liquid chromatography with tandem mass spectrometric detection

    OpenAIRE

    Cai, Min; Liu, Yi-Ming

    2008-01-01

    Salsolinol, 1-methyl-6,7-dihydroxy-2,3,4,5-tetrahydroisoquinoline (SAL), is a precursor of a Parkinsonian neurotoxin, N-methysalsolinol (N-methyl-SAL). Previous studies have shown that individual enantiomers of N-methyl-SAL possess distinct neurotoxicological properties. In this work, a chiral high-performance liquid chromatography (HPLC) method with electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the quantification of (R/S)-SAL enantiomers. Enantiose...

  9. Comparison of Metal and Metal Oxide Media for Phosphopeptide Enrichment Prior to Mass Spectrometric Analyses

    OpenAIRE

    Gates, Matthew B.; Tomer, Kenneth B.; Deterding, Leesa J.

    2010-01-01

    Several affinity resins consisting of ionic metals or metal oxides were investigated for their phosphopeptide enrichment capabilities with subsequent mass spectrometric analyses. Commercially-available enrichment MOAC resins using manufacturer’s and/or published protocols were compared and evaluated for the most efficient and selective method that could be implemented as a standard enrichment procedure. From these comparative analyses using a tryptic digest of casein proteins, it was determin...

  10. Mass Spectrometric Detection of Nanoparticle Host–Guest Interactions in Cells

    OpenAIRE

    Yan, Bo; Yesilbag Tonga, Gulen; Hou, Singyuk; Fedick, Patrick W.; Yeh, Yi-Cheun; Alfonso, Felix S.; Mizuhara, Tsukasa; Vachet, Richard W.; Rotello, Vincent M.

    2014-01-01

    Synthetic host–guest chemistry is a versatile tool for biomedical applications. Characterization and detection of host–guest complexes in biological systems, however, is challenging due to the complexity of the biological milieu. Here, we describe and apply a mass spectrometric method to monitor the association and dissociation of nanoparticle (NP)-based host–guest interactions that integrates NP-assisted laser desorption/ionization (LDI) and matrix assisted laser desoption/ionization (MALDI)...

  11. Mass spectrometric characterization of urinary fibrinogen-derived peptides in prostate cancer and renal cell carcinoma

    OpenAIRE

    Mesihää, M. (Markus)

    2015-01-01

    In previous studies we have found that urinary fibrinogen-derived peptides are potential tumor markers for renal cell carcinoma. These peptides occur at low concentrations in urine. Identification of a low-abundant tumor marker requires optimal sample preparation and a highly sensitive analyzer. In this work different chromatographic and mass spectrometric methods were compared and evaluated for tumor marker discovery. We used urine samples from patients with renal cell carcinoma and pro...

  12. Rapid identification of viridans streptococci by mass spectrometric discrimination.

    Science.gov (United States)

    Friedrichs, C; Rodloff, A C; Chhatwal, G S; Schellenberger, W; Eschrich, K

    2007-08-01

    Viridans streptococci (VS) are responsible for several systemic diseases, such as endocarditis, abscesses, and septicemia. Unfortunately, species identification by conventional methods seems to be more difficult than species identification of other groups of bacteria. The aim of the present study was to evaluate the use of cell matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF-MS) for the rapid identification of 10 different species of VS. A total of 99 VS clinical isolates, 10 reference strains, and 20 strains from our in-house culture collection were analyzed by MALDI-TOF-MS. To evaluate the mass-spectrometric discrimination results, all strains were identified in parallel by phenotypic and genotypic methods. MALDI-TOF-MS identified 71 isolates as the mitis group, 23 as the anginosus group, and 5 as Streptococcus salivarius. Comparison of the species identification results obtained by the MALDI-TOF-MS analyses and with the phenotypic/genotypic identification systems showed 100% consistency at the species level. Thus, MALDI-TOF-MS seems to be a rapid and reliable method for the identification of species of VS from clinical samples. PMID:17553974

  13. Maintenance of stability in γ spectrometric system of low active and environmental samples - a practical experience

    International Nuclear Information System (INIS)

    Particle Accelerators are becoming part of the society with more and more medical and Industrial types are added every year in addition to research type of accelerators. The outflow of materials to the public domain from such accelerator facilities need to checked carefully and must be released after ensuring the activities of such materials should not exceed the regulatory limits. Health Physics Unit, VECC is involved in analyzing food product samples, seized samples which are suspected to contain Uranium etc and other environmental samples in addition to analyzing radioactive materials evolved from Operational Health Physics work. Most of these analyses involve γ Spectrometric Systems of high efficiency and high resolution types. The efficacy of the analysis and results depends on various parameters of the spectrometric system. The electrical noise from the power supply system and other noises picked up, even in the range of a few milli volts range, have been found to affect the stability of the system. These effects may not be present initially during installation but may creep in due course due to various reasons including weather conditions, wear and tear etc. Unless these problems are attended in regular intervals, the stability of the spectrometric systems and hence the results of analysis of the low active and environmental samples, will not be satisfactory. The work describes the practical problems faced by Health Physics Unit, the methods employed in identifying the problems, the necessary remedial measures taken, the final outcome in the stability and the procedures framed in order to avoid in future. (author)

  14. Laser-spectrometric gas analysis: CO2–TDLAS at 2 µm

    International Nuclear Information System (INIS)

    Employing direct absorption spectroscopy and using a spectrometer comprising a single-pass and a multipass white cell, we probed the R(12) line of carbon dioxide (CO2) in the combination band around 2 µm. Gravimetric gas standards containing CO2, between 300 and 60 000 µmol mol−1 (0.03% to 6%), in N2 were quantified by means of the TILSAM method. The spectrometric results were compared with the gravimetric reference values. We describe our implementation of the ‘Guide to the Expression of Uncertainty in Measurements’ to infrared laser-spectrometric gas analysis. Data quality objectives are addressed by uncertainty and traceability flags. Uncertainty budgets are presented to show the quality of the results and to demonstrate software-assisted uncertainty assessment. The relative standard uncertainties of the spectrometrically measured CO2 amount fractions at, e.g., ambient levels of 360 µmol mol−1 and at exhaled breath gas levels of 50 mmol mol−1 were 1.4% and 0.7%, respectively. Our detection limit was 2.2 µmol mol−1. The reproducibility of individual results was in the ±1% range. Furthermore, we measured collisional broadening coefficients of the R(12) line of CO2 at 4987.31 cm−1. The relative standard uncertainties of the measured self-, nitrogen-, oxygen- and air-broadening coefficients were in the ±1.7% range. (paper)

  15. Spectrometric measurements of radioisotope activity in the thyroid

    Science.gov (United States)

    Osko, Jakub; Golnik, Natalia

    2008-01-01

    The results of measurements of iodine 131I and technetium 99mTc uptake in human thyroid, performed with scintillation or semiconductor detectors can exhibit a considerable uncertainty due to the differences in the thyroid position in the patient's neck. Basic physical laws of radiation attenuation and scattering show that the final shape of the registered spectrum should depends on the thyroid position in the neck and on the thickness of the tissue between the thyroid and the detector. The use of the spectrometric measuring method is proposed in this work for determination of the iodine gathering effective depth. The performed studies showed that the measurements results can be used for improving the accuracy of the iodine 131I activity in thyroid measurements and for selection of the group of patients for whom the anatomical position of the thyroid or the spatial distribution of the iodine gathering is much different than the standard one, assumed during the calibration of the counters. The results of the measurements were in agreement with Monte-Carlo calculations of the detector response. The method was used in routine monitoring of occupationally exposed persons, using the thyroid counter. A group of six persons with measurable internal contamination was selected and the measurements were performed on consecutive days, so the results could be registered at decreasing iodine activities in the thyroid. Larger series of measurements were performed at Brodno Regional Hospital in Warsaw, for a group of 95 patients after diagnostic administration of iodine 131I.

  16. Determination of iodine to compliment mass spectrometric measurements

    International Nuclear Information System (INIS)

    The dose of iodine-129 to facility personnel and the general public as a result of past, present, and future activities at DOE sites is of continuing interest, WINCO received about 160 samples annually in a variety of natural matrices, including snow, milk, thyroid tissue, and sagebrush, in which iodine-129 is determined in order to evaluate this dose, Currently, total iodine and the isotopic ratio of iodine-127 to iodine-129 are determined by mass spectrometry. These two measurements determine the concentration of iodine-129 in each sample, These measurements require at least 16 h of mass spectrometer operator time for each sample. A variety of methods are available which concentrate and determine small quantities of iodine. Although useful, these approaches would increase both time and cost. The objective of this effort was to determine total iodine by an alternative method in order to decrease the load on mass spectrometry by 25 to 50%. The preparation of each sample for mass spectrometric analysis involves a common step--collection of iodide on an ion exchange bed. This was the focal point of the effort since the results would be applicable to all samples

  17. Surface acoustic wave nebulization facilitating lipid mass spectrometric analysis.

    Science.gov (United States)

    Yoon, Sung Hwan; Huang, Yue; Edgar, J Scott; Ting, Ying S; Heron, Scott R; Kao, Yuchieh; Li, Yanyan; Masselon, Christophe D; Ernst, Robert K; Goodlett, David R

    2012-08-01

    Surface acoustic wave nebulization (SAWN) is a novel method to transfer nonvolatile analytes directly from the aqueous phase to the gas phase for mass spectrometric analysis. The lower ion energetics of SAWN and its planar nature make it appealing for analytically challenging lipid samples. This challenge is a result of their amphipathic nature, labile nature, and tendency to form aggregates, which readily precipitate clogging capillaries used for electrospray ionization (ESI). Here, we report the use of SAWN to characterize the complex glycolipid, lipid A, which serves as the membrane anchor component of lipopolysaccharide (LPS) and has a pronounced tendency to clog nano-ESI capillaries. We also show that unlike ESI SAWN is capable of ionizing labile phospholipids without fragmentation. Lastly, we compare the ease of use of SAWN to the more conventional infusion-based ESI methods and demonstrate the ability to generate higher order tandem mass spectral data of lipid A for automated structure assignment using our previously reported hierarchical tandem mass spectrometry (HiTMS) algorithm. The ease of generating SAWN-MS(n) data combined with HiTMS interpretation offers the potential for high throughput lipid A structure analysis. PMID:22742654

  18. 脉冲熔融-飞行时间质谱法测定金属材料中氧、氮、氢和氩%Simultaneous Determination of Oxygen, Nitrogen, Hydrogen and Argon in Metals by Pulse Heating and Time of FlightMass Spectrometric Method

    Institute of Scientific and Technical Information of China (English)

    沈学静; 王蓬; 胡少成; 杨植岗; 马红权; 杨倩倩; 高伟; 周振; 王海舟

    2011-01-01

    采用自主研制的脉冲熔融飞行时间质谱法可以固时测定金属中O,N,H和Ar.重点讨论质谱谱线的选择,信号获得以及数据处理和校准,并给出O,N,H和Ar 4种的检出限分别为0.021,0.060,0.002和0.002 μg/g,线性范围分别为0.070~500 μg/g,0.200~400 μg/g,0.006~40 μg/g和0.005~15 μg/g.并利用不同样品对本方法的准确性和精密度进行了验证,实验结果与传统方法吻合.实验表明,本方法准确、有效,可同时测定4种气体元素O,N,H和Ar.%A pulse heating and time of flight-mass spectrometric method was used for quantitative determination of oxygen, nitrogen, hydrogen and argon in metals. The analyzing process was introduced, including mass spectral line selection, signal acquisition, data processing and calibration. The detection limits of (), N, H, Ar are 0. 021, 0. 060, 0. 002, 0. 002 μg/g, and the linear ranges of (), N, H, Ar are 0.070 -500, 0.200 - 400, 0.006 - 40, 0.005 - 15 μg/g, respectively. The accuracy and precision of the method have also been verified by analyzing several kinds of samples. The results are consistent with those of traditional method, which shows that the new method is sensitive and efficient.

  19. Extraction-mass spectrometric determination of platinum metals in materials of complex composition

    International Nuclear Information System (INIS)

    A method is developed for the extraction mass-spectrometric determination of platinum metals, including ruthenium. The loWer limit of detectable contents is 1.6x10-6 mass.% (a coefficient of concentration is 50). The relative standard deviation is 0.19-0.38. Relative sensitivity coefficients determined experimentally with the aid of reference samples for platinum metals enable the systematic errors of analysis results to be taken into account. The method is most advisably used for the simultaneous determination of platinum metals in complex objects (minerals, rocks, etc.)

  20. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    The standard covers analytical procedures to determine compliance of nuclear-grade boron carbide powder and pellets to specifications. The following methods are described in detail: total carbon by combustion and gravimetry; total boron by titrimetry; isotopic composition by mass spectrometry; chloride and fluoride separation by pyrohydrolysis; chloride by constant-current coulometry; fluoride by ion-selective electrode; water by constant-voltage coulometry; impurities by spectrochemical analysis; soluble boron by titrimetry; soluble carbon by a manometric measurement; metallic impurities by a direct reader spectrometric method. (JMT)

  1. Mass Spectrometric Immunoassays in Characterization of Clinically Significant Proteoforms

    Directory of Open Access Journals (Sweden)

    Olgica Trenchevska

    2016-03-01

    Full Text Available Proteins can exist as multiple proteoforms in vivo, as a result of alternative splicing and single-nucleotide polymorphisms (SNPs, as well as posttranslational processing. To address their clinical significance in a context of diagnostic information, proteoforms require a more in-depth analysis. Mass spectrometric immunoassays (MSIA have been devised for studying structural diversity in human proteins. MSIA enables protein profiling in a simple and high-throughput manner, by combining the selectivity of targeted immunoassays, with the specificity of mass spectrometric detection. MSIA has been used for qualitative and quantitative analysis of single and multiple proteoforms, distinguishing between normal fluctuations and changes related to clinical conditions. This mini review offers an overview of the development and application of mass spectrometric immunoassays for clinical and population proteomics studies. Provided are examples of some recent developments, and also discussed are the trends and challenges in mass spectrometry-based immunoassays for the next-phase of clinical applications.

  2. Single-Laboratory Validation of a High-Performance Liquid Chromatographic-Diode Array Detector-Fluorescence Detector/Mass Spectrometric Method for Simultaneous Determination of Water-Soluble Vitamins in Multivitamin Dietary Tablets

    OpenAIRE

    Chen, Pei; Atkinson, Renata; Wolf, Wayne R.

    2009-01-01

    The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors [diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS)] for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phas...

  3. Aeromagnetic and gamma spectrometric interpretation of the Riacho Queimadas sheet

    International Nuclear Information System (INIS)

    This paper presents the aeromagnetic and gamma-spectrometric interpretation of the Riacho Queimadas Sheet (SC.24-V-A-I), southeastern Piaui State, Brazil, originated from studies as part of the Programa Levantamentos Geologicos Basicos do Brasil-PLGB (basic Geological Surveying Program of Brazil). The interpretation of magnetometric and gamma-spectrometric maps identified mafic-ultramafic and felsic terrains and sedimentary rocks and the utilization of modelling techniques defined the shape and variation in thickness of geologic bodies. It was possible to limit young igneous intrusive rocks and to suggest the hierarchy of structural alignments and shear zones, based on anomalies shape analyses. (author)

  4. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    International Nuclear Information System (INIS)

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  5. Cross-validation of a mass spectrometric-based method for the therapeutic drug monitoring of irinotecan: implementation of matrix-assisted laser desorption/ionization mass spectrometry in pharmacokinetic measurements.

    Science.gov (United States)

    Calandra, Eleonora; Posocco, Bianca; Crotti, Sara; Marangon, Elena; Giodini, Luciana; Nitti, Donato; Toffoli, Giuseppe; Traldi, Pietro; Agostini, Marco

    2016-07-01

    Irinotecan is a widely used antineoplastic drug, mostly employed for the treatment of colorectal cancer. This drug is a feasible candidate for therapeutic drug monitoring due to the presence of a wide inter-individual variability in the pharmacokinetic and pharmacodynamic parameters. In order to determine the drug concentration during the administration protocol, we developed a quantitative MALDI-MS method using CHCA as MALDI matrix. Here, we demonstrate that MALDI-TOF can be applied in a routine setting for therapeutic drug monitoring in humans offering quick and accurate results. To reach this aim, we cross validated, according to FDA and EMA guidelines, the MALDI-TOF method in comparison with a standard LC-MS/MS method, applying it for the quantification of 108 patients' plasma samples from a clinical trial. Standard curves for irinotecan were linear (R (2) ≥ 0.9842) over the concentration ranges between 300 and 10,000 ng/mL and showed good back-calculated accuracy and precision. Intra- and inter-day precision and accuracy, determined on three quality control levels were always <12.8 % and between 90.1 and 106.9 %, respectively. The cross-validation procedure showed a good reproducibility between the two methods, the percentage differences within 20 % in more than 70 % of the total amount of clinical samples analysed. PMID:27235158

  6. A straightforward, quantitative ultra-performance liquid chromatography-tandem mass spectrometric method for heparan sulfate, dermatan sulfate and chondroitin sulfate in urine: an improved clinical screening test for the mucopolysaccharidoses.

    Science.gov (United States)

    Zhang, Haoyue; Wood, Tim; Young, Sarah P; Millington, David S

    2015-02-01

    Mucopolysaccharidoses (MPS) are complex storage disorders that result in the accumulation of glycosaminoglycans (GAGs) in urine, blood, brain and other tissues. Symptomatic patients are typically screened for MPS by analysis of GAG in urine. Current screening methods used in clinical laboratories are based on colorimetric assays that lack the sensitivity and specificity to reliably detect mild GAG elevations that occur in some patients with MPS. We have developed a straightforward, reliable method to quantify chondroitin sulfate (CS), dermatan sulfate (DS) and heparan sulfate (HS) in urine by stable isotope dilution tandem mass spectrometry. The GAGs were methanolyzed to uronic acid-N-acetylhexosamine or iduronic acid-N-glucosamine dimers and mixed with stable isotope labeled internal standards derived from deuteriomethanolysis of GAG standards. Specific dimers derived from HS, DS and CS were separated by ultra-performance liquid chromatography and analyzed by electrospray ionization tandem mass spectrometry using selected reaction monitoring for each targeted GAG product and its corresponding internal standard. The method was robust with a mean inaccuracy from 1 to 15%, imprecision below 11%, and a lower limit of quantification of 0.4mg/L for CS, DS and HS. We demonstrate that the method has the required sensitivity and specificity to discriminate patients with MPS III, MPS IVA and MPS VI from those with MPS I or MPS II and can detect mildly elevated GAG species relative to age-specific reference intervals. This assay may also be used for the monitoring of patients following therapeutic intervention. Patients with MPS IVB are, however, not detectable by this method. PMID:25458519

  7. A new reversed-phase liquid chromatographic/tandem mass spectrometric method for analysis of underivatised amino acids: evaluation for the diagnosis and the management of inherited disorders of amino acid metabolism.

    Science.gov (United States)

    Piraud, M; Vianey-Saban, C; Bourdin, C; Acquaviva-Bourdain, C; Boyer, S; Elfakir, C; Bouchu, D

    2005-01-01

    Seventy-six compounds of biological interest for the diagnosis of inherited disorders of amino acids (AA) metabolism have previously been demonstrated to be detectable in positive mode electrospray ionisation tandem mass spectrometry (ESI-MS/MS), after separation by ion-pairing reversed-phase liquid chromatography (RPLC). The separation method used tridecafluoroheptanoic acid as ion-pairing agent, and a gradient of acetonitrile for the elution of the most retained compounds. This method had previously been demonstrated to be suitable for the qualitative diagnosis of many AA disorders, and for the quantitative measurement of 16 AA in biological fluids, using their stable isotope labelled (SIL) AA as internal standard. For quantification of the other AA, an internal standard was chosen among the available SIL-AA, as close as possible to the analyte to be measured, in terms of structural analogy, and of retention time in the chromatographic system. The performances of the quantitative analysis of the other AA to be measured are reported here. They show validated results for several AA, allowing their accurate quantification, with another SIL-AA as internal standard. For some other AA, quantitative results were not accurate, allowing only semi-quantitative or qualitative determination for these parameters. PMID:16235234

  8. Electrothermal atomization atomic absorption spectrometric determination of trace metals in uranium-plutomium fuel materials

    International Nuclear Information System (INIS)

    Atomic absorption spectrometric methods using the electrothermal mode of atomization developed for the determination of Ag, Be, Ca, Cd, Cr, Co, Cu, Fe, Li, Mn, Na, Ni, Sn and Zn in (U, Pu) solution with 4% plutonium have been described. The carbon rod atomizer has been adapted for glove box operation to enable handling of plutonium containing solution samples. Multielement solution standards with graded concentrations of the analytes and fixed concentration of the matrix are used in the standardization process. Nanogram to sub-nanogram quantities of the analytes have been determined with a precision of better than 9% RSD using 5 μl of the sample aliquots. (orig.)

  9. Development of resin-bead isotope-dilution mass spectrometric techniques for Tc-99 analysis

    International Nuclear Information System (INIS)

    An isotope dilution mass spectrometric method was developed for the analysis of Tc-99 after isolating it onto anion exchange resin beads. A single resin bead containing Tc-99 and Tc-97 spike is loaded onto a rhenium V-shaped filament for thermal emission mass spectrometry. The application of this technique requires the use of a mass spectrometer of high abundance sensitivity and pulse counting capability for the necessary ion detection sensitivity. This paper discusses the development of the technique, including the mass spectrometer, choice of filament material, scanning modes, interferences, and present achievable sample sensitivities

  10. Experimental control of burn-up calculations for high temperature reactor fuel by introduction of a special alpha spectrometric method for the determination of transuranium content. An attempt to establish isotopic correlations

    International Nuclear Information System (INIS)

    In the field of high-temperature-reactor (HTR) fuel investigation there is a great interest in the experimental and calculational determination of heavy metal content under the aspects of burn-up physics and for the prediction of reliable data for reprocessing and waste management. Using a laser-micro-boring preparation method, high resolution alpha-spectroscopy and sophisticated computer decomposition programs we identify qualitatively and quantitatively most of the important actinide isotopes in irradiated HTR-fuel. Additionally we use data, delivered by gamma- and mass-spectroscopy of the same fuel samples. The evaluated results are compared with calculational results from the burn-up code ORIGEN, using a special generated HTR-neutron-cross-section library. In a first step we determine new cross sections for the uranium and plutonium isotopes depending on the irradiation conditions. In a second step we calculate correlations between the heavy metal isotopes and the burn-up or the fission products

  11. Development and validation of an ultra-high-performance liquid chromatography tandem mass spectrometric method for the simultaneous determination of free and conjugated Alternaria toxins in cereal-based foodstuffs.

    Science.gov (United States)

    Walravens, Jeroen; Mikula, Hannes; Rychlik, Michael; Asam, Stefan; Ediage, Emmanuel Njumbe; Di Mavungu, José Diana; Van Landschoot, Anita; Vanhaecke, Lynn; De Saeger, Sarah

    2014-10-31

    A UPLC-ESI(+/-)-MS/MS method for the simultaneous determination of free (alternariol, alternariol monomethyl ether, altenuene, tenuazonic acid, tentoxin, altertoxin-I) and conjugated (sulfates and glucosides of alternariol and alternariol monomethyl ether) Alternaria toxins in cereals and cereal products (rice, oat flakes and barley) was developed. Optimization of the sample preparation and extraction methodology was achieved through experimental design, using full factorial design for extraction solvent composition optimization and fractional factorial design to identify the critical factors in the sample preparation protocol, which were in turn subjected to optimization. Final extracts were analysed using an Waters Acquity UPLC system coupled to a Quattro Premier XE mass spectrometer equipped with an electrospray interface operated in both positive and negative ionization mode. Chromatographic separation was achieved using an Acquity UPLC HSS T3 column, and the applied gradient elution programme allowed for the simultaneous determination of 10 Alternaria toxins in a one-step chromatographic run with a total run time of only 7min. Subsequently, the method, applying isotopically labelled internal standards ([(2)H4]-alternariol monomethyl ether and [(13)C6,(15)N]-tenuazonic acid), was validated for several parameters such as linearity, apparent recovery, limit of detection, limit of quantification, precision, measurement uncertainty and specificity (in agreement with the criteria mentioned in Commission Regulation No. 401/2006/EC and Commission Decision No. 2002/657/EC). During validation, quality of the bioanalytical data was improved by counteracting the observed heteroscedasticity through the application of weighted least squares linear regression (WLSLR). Finally, 24 commercially available cereal-based foodstuffs were subjected to analysis, revealing the presence of tenuazonic acid in both rice and oat flake samples (

  12. Preparation and spectrometric identification of amide derivatives with antimalaric

    International Nuclear Information System (INIS)

    The structures of polymeric compounds using spectrometric analysis of infrared, ultraviolet and protonic magnetic resonance and 13C nuclear magnetic resonance are studied. Some structural models are used such as antimalaric-sulfones and pyrimidinic derivatives, and non-polymeric derivatives of active compounds. A comparative analysis on structures less complexes is shown. (M.J.C.). Spectrums 186 p

  13. Recent advances in mass spectrometric applications in hydrology

    International Nuclear Information System (INIS)

    The recent advances in mass spectrometric applications in hydrology include 18O of nitrates and sulphates, 37Cl of chlorides for studying origin of groundwater pollution, 3He/4He for geothermal fluids and analysis, 14C, 36Cl and 129I for dating groundwater by Accelerator Mass Spectrometry (AMS)

  14. Assessment of current mass spectrometric workflows for the quantification of low abundant proteins and phosphorylation sites

    Directory of Open Access Journals (Sweden)

    Manuel Bauer

    2015-12-01

    Full Text Available The data described here provide a systematic performance evaluation of popular data-dependent (DDA and independent (DIA mass spectrometric (MS workflows currently used in quantitative proteomics. We assessed the limits of identification, quantification and detection for each method by analyzing a dilution series of 20 unmodified and 10 phosphorylated synthetic heavy labeled reference peptides, respectively, covering six orders of magnitude in peptide concentration with and without a complex human cell digest background. We found that all methods performed very similarly in the absence of background proteins, however, when analyzing whole cell lysates, targeted methods were at least 5–10 times more sensitive than directed or DDA methods. In particular, higher stage fragmentation (MS3 of the neutral loss peak using a linear ion trap increased dynamic quantification range of some phosphopeptides up to 100-fold. We illustrate the power of this targeted MS3 approach for phosphopeptide monitoring by successfully quantifying 9 phosphorylation sites of the kinetochore and spindle assembly checkpoint component Mad1 over different cell cycle states from non-enriched pull-down samples. The data are associated to the research article ‘Evaluation of data-dependent and data-independent mass spectrometric workflows for sensitive quantification of proteins and phosphorylation sites׳ (Bauer et al., 2014 [1]. The mass spectrometry and the analysis dataset have been deposited to the ProteomeXchange Consortium (http://proteomecentral.proteomexchange.org via the PRIDE partner repository with the dataset identifier PXD000964.

  15. Single hair cocaine consumption monitoring by mass spectrometric imaging.

    Science.gov (United States)

    Porta, Tiffany; Grivet, Chantal; Kraemer, Thomas; Varesio, Emmanuel; Hopfgartner, Gérard

    2011-06-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI-MSI) was used to image the distribution of cocaine and its metabolites in intact single hair samples from chronic users down to a concentration of 5 ng/mg. Acquisitions were performed in rastering mode, at a speed of 1 mm/s and in the selected reaction monitoring (SRM) mode on a MALDI triple quadrupole linear ion trap fitted with a high repetition rate laser (1 kHz). Compared to traditional methods based on LC-MS/MS or GC-MS(/MS) which require to segment the hair to obtain spatial resolution, MALDI-MSI, with a straightforward sample preparation beforehand, allowed obtaining a spatial resolution of 1 mm and thus the chronological information about cocaine consumption contained in a single intact hair over several months could be monitored. The analysis time of an intact single hair sample of 6 cm is approximately of 6 min. Cocaine and its metabolites benzoylecgonine, ethylcocaine, and norcocaine were investigated in nine sets of hair samples for forensic purposes. The analyses were accomplished by spraying α-cyano-4-hydroxycinnamic acid (CHCA), 4-chloro-α-cyano-cinnamic acid (Cl-CCA), or (E)-2-cyano-3-(naphthalen-2-yl)acrylic acid (NpCCA) as MALDI matrices. We also propose a rapid strategy for sensitive confirmatory analyses with both MS/MS and MS(3) experiments performed directly on intact hair samples. Since only part of the hair strand is analyzed, additional analyses are possible at any time on the remaining hair from the strand. PMID:21510611

  16. 邻菲啰啉-Fe^3+分光光度法测定食品中的亚硫酸盐%A Spectrometric Method for Sulfite Determination Using the System of Complex of Phenanthroline and Fe~(3+)

    Institute of Scientific and Technical Information of China (English)

    廖文生; 刘中勇; 赵群; 谢思瑶; 伍冠红

    2012-01-01

    Phenanthroline can interact with Fe3+ and Fe2+ to form metal complexes of different colors.Phenanthroline-Fe3+ was changed to phenanthroline-Fe2+ due to the redox reaction between sulfite and Fe3+ with dramatic spectrum changes.Based on this,a spectrometric method for the determination of sulfite was developed.In pH5.00 NaAc-HAc buffer,the addition of sulfite to the phenanthroline-Fe3+ system results in significant absorption increase at 510 nm which is proportional to the concentration of sulfite over the range of 1.08 ×10-6-1.60 ×10-5mol/L with a limit of detection of 1.08×10-7mol/L.The proposed method was applied to determine sulfite in biscuits,the recovery being 92.2%-101.8%.%邻菲啰啉可与Fe3+和Fe2+结合形成不同颜色的金属配合物。利用亚硫酸对Fe3+离子的还原作用,使邻菲啰啉-Fe3+配合物转化为邻菲啰啉-Fe2+,产生显著的光谱变化,据此建立测定亚硫酸盐的光谱分析法。研究结果显示,在pH5.00的乙酸钠-乙酸缓冲溶液中,亚硫酸盐的加入使体系在510 nm处的吸光度显著增强,在一定浓度范围内510nm处吸光度的增加值与亚硫酸盐浓度呈良好线性关系,其线性范围为1.08×10-6-1.60×10-5mol/L,检测限为1.08×10-7mol/L。本方法用于测定饼干中的亚硫酸盐,回收率为92.2%-101.8%。

  17. Particle size independent spectrometric determination of wear metals in aircraft lubricating oils

    International Nuclear Information System (INIS)

    A method for the particle size independent determination of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti in synthetic ester lubricating oils by spectrometric analysis is presented. Partial dissolution of Cr, Si, Pb, and Ag also occurs. Used ester lubricating oils as well as samples prepared with -325 mesh (44 μm) or -200 mesh (74 μm) metal powders were reacted with a small amount of hydrofluoric acid and aqua regia at 650C for 45 min with ultrasonic agitation. The reacted mixture was then diluted with a methyl isobutyl ketone and isopropyl alcohol mixture and analyzed spectrometrically. The recoveries for metal powder suspensions of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti ranged from 97 to 103% and the relative standard deviation ranged from 4 to 10%. In addition to the metal powder suspensions, over 200 aircraft oil samples were analyzed. The method is much faster and more convenient than previously reported particle size independent methods using ashing techniques

  18. Study of the spectrometric performances of monolithic CdZnTe / CdTe gamma ray detectors

    International Nuclear Information System (INIS)

    Pixelated monolithic CdTe/CdZnTe semiconductor gamma ray detectors are brought to replace scintillation detectors for medical applications, notably for single photon emission computed tomography (SPECT). In addition to compactness, they present better spectrometric performances: energy resolution, detection efficiency, and spatial resolution. Moreover, the photons depth of interaction in the crystal can be measured. This work aimed in studying experimentally and by simulation the correlations between anodes pitch, material physic properties (resistivity and electron transport properties), and detectors spectrometric performances. We have compared several methods of measuring the photon interaction depth, and have obtained an energy resolution ranging from 1.7% to 7% at 122 keV, according to material, for 5 mm thick detectors. Charge sharing between adjacent anodes has been studied and a measured data processing is proposed. (author)

  19. Quantitative analysis of flavonols, flavones, and flavanones in fruits, vegetables and beverages by high-performance liquid chromatography with photo-diode array and mass spectrometric detection

    DEFF Research Database (Denmark)

    Justesen, U.; Knuthsen, Pia; Leth, Torben

    A high-performance liquid chromatographic (HPLC) separation method viith photo-diode array (PDA) and mass spectrometric (MS) detection was developed to determine and quantify flavonols, flavones, and flavanones in fruits, vegetables and beverages. The compounds were analysed as aglycones, obtained...

  20. Analysis of Polar Lipids in Chlamydomonas reinhardtii Using Nanoelectrospray Direct Infusion Method and Gas Chromatography and Mass Spectrometric Detection%基于芯片的直接进样质谱法和气相色谱-质谱测定莱茵衣藻中的极性脂类

    Institute of Scientific and Technical Information of China (English)

    杨大伟; 范晓蕾; Kind Tobias; Fiehn Oliver; 郭荣波

    2013-01-01

    . reinhardtii. Among them, twenty classes of diacylglyceryltrimethylhomoserine that are very special lipid species in C. reinhardtii belonging to betaine lipids were annotated with in-house Lipidblast database. In order to validate this Lipidblast match, we performed a manual spectral interpretation of every experimental MS/MS spectrum to ensure authentic ester annotations. Besides, we also applied a gas chromatography tandem mass spectrometric method to detect free fatty acids in C. reinhardtii and found that linolenic acid, linoleic acid and palmitic acid are most abundant free fatty acids in C. reinhardtii. This study provides a potential comprehensive lipidomic method for further lipid analysis in algal research.

  1. The 3D inversion of airborne gamma-ray spectrometric data

    Science.gov (United States)

    Minty, Brian; Brodie, Ross

    2016-07-01

    We present a new method for the inversion of airborne gamma-ray spectrometric line data to a regular grid of radioelement concentration estimates on the ground. The method incorporates the height of the aircraft, the 3D terrain within the field of view of the spectrometer, the directional sensitivity of rectangular detectors, and a source model comprising vertical rectangular prisms with the same horizontal dimensions as the required grid cell size. The top of each prism is a plane surface derived from a best-fit plane to the digital elevation model of the earth's surface within each grid cell area. The method is a significant improvement on current methods, and gives superior interpolation between flight lines. It also eliminates terrain effects that would normally remain in the data after the conventional processing of these data assuming a flat-earth model.

  2. Mass Spectrometric Analysis of Water-soluble Gold Nanoclusters

    International Nuclear Information System (INIS)

    Batches of water-soluble gold nanoclusters of nominal 2.0 or 3.5-nm diameter were prepared to evaluate particle size determinations by a number of techniques such as transmission electron microscopy or atomic force microscopy and to validate estimates derived by mass spectrometric analysis using matrix-assisted laser desorption ionization (MALDI). Good agreement was found and MALDI lends itself to analyses even in the presence of aggregates

  3. Challenges and recent advances in mass spectrometric imaging of neurotransmitters

    OpenAIRE

    Gemperline, Erin; Chen, Bingming; Li, Lingjun

    2014-01-01

    Mass spectrometric imaging (MSI) is a powerful tool that grants the ability to investigate a broad mass range of molecules, from small molecules to large proteins, by creating detailed distribution maps of selected compounds. To date, MSI has demonstrated its versatility in the study of neurotransmitters and neuropeptides of different classes toward investigation of neurobiological functions and diseases. These studies have provided significant insight in neurobiology over the years and curre...

  4. System for Gamma an X rays fluorescence spectrometric

    International Nuclear Information System (INIS)

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  5. MALDI mass spectrometric imaging meets "omics": recent advances in the fruitful marriage.

    Science.gov (United States)

    Crecelius, A C; Schubert, U S; von Eggeling, F

    2015-09-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI MSI) is a method that allows the investigation of the molecular content of surfaces, in particular, tissues, within its morphological context. The applications of MALDI MSI in the field of large-scale mass spectrometric studies, which are typically denoted by the suffix "omics", are steadily increasing. This is because, on the one hand, technical advances regarding sample collection and preparation, matrix application, instrumentation, and data processing have enhanced the molecular specificity and sensitivity of MALDI MSI; on the other hand, the focus of the "omics" community has moved from establishing an inventory of certain compound classes to exploring their spatial distribution to gain novel insights. Thus, the aim of this mini-review is twofold, to display the state-of-the-art in terms of technical aspects in MALDI MSI and to highlight selected applications in the last two years, which either have significantly advanced a certain "omics" field or have introduced a new one through pioneering efforts. PMID:26161715

  6. New miniaturized alpha/beta spectrometric systems for the surface contamination monitoring and radon personal dosimeter

    International Nuclear Information System (INIS)

    We report on a new miniaturized alpha/beta spectrometric system. This cheque cart 12 bit SARAD spectra 5011 spectrometric system we can combine with a new developed detector, preamp and forming unit. A very important application of this new measuring system is the alpha nuclidspecific surface contamination monitoring. Especially in old nuclear power station it is very important in the decommissioning process to know the nuclide vector. We report of applications to use this new technology to measure the nuclide vector in old lead cells or construction elements in old nuclear reactors. We measure surface contamination in the order of 1 Bq/cm2 of Pu-239 very easy. A other modification of this cheque cart spectrometer is the radon personal dosimeter. In this case we have integrated on a cheque cart a 8 bit spectrometer, a 1cm2 silicon detector, the signal processing, AD-conversion, data storage and transponder system for the data transfer. Using this transponder system we can also use a local resoluted dosimetry. The main application of this system is the radon dosimetry on workplaces, for instance water works, mines, show caves and other work places with high radon levels. This easy system can replace the passive screening methods and also the nuclear track etch dosimeters. Because the low price and the easy data read out the amortisation of such a electronic system is in the order of two years

  7. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    International Nuclear Information System (INIS)

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U+ , UO+ and UO2+ ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  8. Mass spectrometric detection, identification, and fragmentation of arseno-phytochelatins.

    Science.gov (United States)

    Schmied-Tobies, Maria I H; Arroyo-Abad, Uriel; Mattusch, Jürgen; Reemtsma, Thorsten

    2014-11-01

    Phytochelatins (PC) are cystein-rich oligopeptides in plants for coordination with toxic metals and metalloids via their thiol groups. The composition, structure, and mass spectrometric fragmentation of arseno-PC (As-PC) with PC of different degree of oligomerization (PC2-PC5) in solution were studied using liquid chromatography coupled in parallel to inductively coupled plasma mass spectrometry and electrospray ionization quadrupole time-of-flight mass spectrometry. As-PC were detected from As(PC2) to As(PC5) with an increasing number of isomers that differ in the position of thiol groups bound to As. Thermodynamic modeling supported the identification process in case of these isomers. Mass spectrometric fragmentation of the As-PC does not follow the established pattern of peptides but is governed by the formation of series of As-containing annular cations, which coordinate to As via S, N, or O. Structure proposals for 30 As-PC fragment ions in the range m/z 147.92 to m/z 1290.18 are elaborated. Many of these fragment ions are characteristic to several As-PC and may be suited for a screening for As-PC in plant extracts. The mass spectrometric data offer the perspective for a future more sensitive determination of As-PC by means of liquid chromatography tandem mass spectrometry with multiple reaction monitoring. PMID:25395130

  9. Mass-spectrometric online monitoring of metabolism for estimation of adequacy of anesthesia

    Science.gov (United States)

    Elizarov, A. Yu.; Levshankov, A. I.; Faizov, I. I.; Shchegolev, A. V.

    2012-08-01

    The possibility of using a mass-spectrometric method for estimation of the adequacy of anesthesia has been demonstrated. The method is based on online monitoring of metabolism by determining the CO2/O2 concentration ratio during expiration in each breathing cycle, which allows the patient's response to surgical injury in the course of total anesthesia to be evaluated. The proposed method has been clinically tested using an electron-impact ionization mass spectrometer connected to the breathing circuit of an inhalation anesthesia machine. It is shown that, using this technique, the time of the patient's organism response to drug correction of the adequacy of lung ventilation during anesthesia can be monitored online.

  10. 运用HPLC-MS对鸦胆子油自微乳给药系统肠吸收的研究%High-performance Liquid Chromatography Coupled with Mass Spectrometric Method for the Intestinal Absorption Study of Brucea Javanica Oil SMEDDS

    Institute of Scientific and Technical Information of China (English)

    陈瑾瑾; 张懿; 王睿锐; 李盈; 沈琦; 马依然

    2012-01-01

    Objective: To develop a rapid, sensitive and selective high-performance liquid chromatography coupled with mass spectrometric method (HPLC-MS) for detection oleic acid and linoleic acid. Methods: The chromatographic separation was achieved on C18 column at 35℃, with a mobile phase consisting of methanol-distilled water (95:5, v/v) at a flow rate of 0.4 mL/min. An in-vitro diffusion chamber system across isolated rat intestinal membranes was chosen as a model. A self-microemulsifying drug delivery system was used to enhance the intestinal absorption of bruces javanica oil. Results: Oleic acid and linoleic acid were separated with retention times of 10.46 ± 0.02 and 8.55 ± 0.01 min, respectively. A good linear relationship for oleic acid and linoleic acid were in the range of 0.50~50.0 ng/mL(oleic acid) and 5.06~101.2 ng/mL(linoleic acid) , respectively. The mean absolute recoveries of oleic acid and linoleic acid determined in middle concentrations were 97.49± 3.11 % and 105.76± 3.13 % respectively. The coefficients of variation for inter-day and intra-day assay were less than 5 %. The absorption of oleic acid and linoleic acid in bruces javanica oil were 2.8-fold and 4.1-fold enhancement in the presence of the self-microemulsifying drug delivery system respectively, compared with brucea javanica oil alone. Conclusion: HPLC-MS method will be of great utility in routine quality control procedure for the determination of oleic acid and linoleic acid in absorption experiments.%目的:建立高效液相色谱-串联质谱法检测油酸和亚油酸含量的方法,从而对鸦胆子油自微乳给药系统中鸦胆子油的肠吸收进行研究.方法:以甲醇-水(95∶5 v/v)为流动相,流速为0.4 mL/min,柱温为35℃作为高效液相色谱的检测条件.利用大鼠小肠膜建立体外药物扩散体系研究鸦胆子油的肠吸收特性.结果:油酸和亚油酸的保留时间分别为10.46± 0.02和8.55±0.01 min,线性范围分别为0.50~50.0 ng

  11. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    International Nuclear Information System (INIS)

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here

  12. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  13. Liquid chromatography-mass spectrometric determination of rufinamide in low volume plasma samples.

    Science.gov (United States)

    Gáll, Zsolt; Vancea, Szende; Dogaru, Maria T; Szilágyi, Tibor

    2013-12-01

    Quantification of rufinamide in plasma was achieved using a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method. The chromatographic separation was achieved on a reversed phase column (Zorbax SB-C18 100mm×3mm, 3.5μm) under isocratic conditions. The mobile phase consisted of a mixture of water containing 0.1% formic acid and methanol (50:50, v/v). The mass spectrometric detection of the analyte was in multiple reaction monitoring mode (MRM) using an electrospray positive ionization (ESI positive). The monitored ions were 127m/z derived from 239m/z rufinamide and 108m/z derived from 251m/z the internal standard (lacosamide). Protein precipitation with methanol was applied for sample preparation using only 50μl aliquots. The concentration range was 40-2000ng/ml for rufinamide in plasma. The limit of detection was 1.25ng/ml and the lower limit of quantification was established at 5ng/ml rufinamide concentration. Selectivity and matrix effect was verified using individual human, rat and rabbit plasma samples. Short-term, post-preparative and freeze-thaw stability was also investigated. The proposed method provides accuracy, precision and high-throughput (short runtime 4.5min) for quantitative determination of rufinamide in plasma. This is the first reported liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for analysis of rufinamide from low volume plasma samples. The LC-MS/MS method was validated according to the current official guidelines and can be applied to accurately measure rufinamide level of large number of plasma samples from clinical studies or therapeutic drug monitoring. PMID:24140655

  14. Development of a dosimetric system using spectrometric technique suitable for operational radiation dose measurements and evaluation

    International Nuclear Information System (INIS)

    The system of quantities and units of radiation and measurements has rapidly progressed in the radiation protection fields, corresponding to the concept reflecting the radiation sensitivity and effects to human body. Usually dosimetric devises are calibrated by using a standard source that satisfies traceability on exposure or absorbed dose, and the value of the quantity that it is intended to measure is obtained by using calculated conversion factors, or the devises adjusted to be proportional to the quantity are employed. But the present concept doesn't accord fully with these recent variability of dose and dosimetry system. Under these circumstances the Spectrometric techniques are expected to be applied most flexibly to dose measurements in compliance with the present dose concept, because information on radiation energy can improve the reliability of dose measurements. The two spectrometric techniques for dose measurements using NaI(Tl) scintillation detector are known in Japan, the one is a Spectrum-to-Dose conversion operator method (G(E) function method), and the other is an unfolding method using a response function array of the detector. These two techniques are practically used in routine environmental gamma radiation monitoring, but in the latter case the accuracy of response functions and the energy resolution are insufficient even in the present situation. In order to improve these points in spectrometric method using NaI(Tl) scintillation detector we have developed a computer program for generating accurate response functions for each incident photon energy of 10 keV intervals. Original standard pulse height spectra for selected monoenergetic photon energy were theoretically calculated by Monte Carlo method and they were decomposed into its constituent components of each interaction. Then, the parameters and shapes of constituent spectra were interpolated in the range from 40 keV to 3.4 MeV. A developed computer program can generate accurate response

  15. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, impurity content. The following analytical procedures, which are described in detail, are designed to show whether or not a given material meets specifications: uranium by ferrous sulfate reduction in phosphoric acid and dichromate titration method; uranium and oxygen uranium atomic ratio by the ignition (gravimetric) impurity correction method; oxygen to uranium atomic ratios by the polarographic method; carbon (total) by direct combustion-thermal conductivity method; total chlorine and fluorine by pyrohydrolysis ion-selective electrode method; moisture by the coulometric, electrolytic moisture analyzer method; nitrogen by the Kjeldahl method; total sulfur by distillation-spectrophotometric method; isotopic uranium composition by multiple-filament surface-ionization mass spectrometric method; spectrochemical determination of trace elements in high-purity uranium dioxide; volatile fluoride impurities by spectrochemical method using the rotating-disk spark technique; spectrochemical determination of silver by gallium oxide carrier D-C arc technique; rare earths by copper spark-spectrochemical method; impurity elements by a spark-source mass spectrographic method; surface area by nitrogen absorption method; total gas in reactor-grade uranium dioxide pellets; thorium and rare earth elements by spectroscopy; hydrogen by inert gas fusion; and uranium isotopic analysis by mass spectrometry. (JMT)

  16. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    International Nuclear Information System (INIS)

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, impurity content. The following analytical procedures, which are described in detail, are designed to show whether or not a given material meets specifications: uranium by ferrous sulfate reduction in phosphoric acid and dichromate titration method; uranium and oxygen uranium atomic ratio by the ignition (gravimetric) impurity correction method; oxygen to uranium atomic ratios by the polarographic method; carbon (total) by direct combustion-thermal conductivity method; total chlorine and fluorine by pyrohydrolysis ion-selective electrode method; moisture by the coulometric, electrolytic moisture analyzer method; nitrogen by the Kjeldahl method; total sulfur by distillation-spectrophotometric method; isotopic uranium composition by multiple-filament surface-ionization mass spectrometric method; spectrochemical determination of trace elements in high-purity uranium dioxide; volatile fluoride impurities by spectrochemical method using the rotating-disk spark technique; spectrochemical determination of silver by gallium oxide carrier D-C arc technique; rare earths by copper spark-spectrochemical method; impurity elements by a spark-source mass spectrographic method; surface area by nitrogen absorption method; total gas in reactor-grade uranium dioxide pellets; thorium and rare earth elements by spectroscopy; hydrogen by inert gas fusion; and uranium isotopic analysis by mass spectrometry

  17. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  18. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    International Nuclear Information System (INIS)

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C18 column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole

  19. Time and spectrometric parameters of photomultiplier 85 and photomultiplier 87

    International Nuclear Information System (INIS)

    A light-pulse generator using a type AL102B light-emitting diode has been used to investigate the temporal and spectrometric parameters of the small FEU-85 and FEU-87 photomultipliers. It was found that the time resolution of the FEU-85 and FEU-87 may be improved by 20-50% through suitable choice of the individual voltage divider. It has been shown that the time and amplitude resolution of the FEU-85 is inversely proportional to the square root of the number of photoelectrons over a wide range of illumination intensities

  20. Mass spectrometric imaging of ginsenosides localization in Panax ginseng root

    OpenAIRE

    Taira, Shu; Ikeda, Ryuzo; Yokota, Naohiko; OSAKA, Issey; Sakamoto, Manabu; Kato, Mitsuro; Sahashi, Yuko

    2010-01-01

    We succeeded in performing mass spectrometric imaging (MSI) of the localization of ginsenosides (Rb_1, Rb_2 or R_c, and Rf) in cross-sections of the Panax ginseng root at a resolution of 100 μm using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Tandem mass spectrometry (MS/MS) of alkali metal-adducted ginsenoside ions revealed structural information of the corresponding saccharides and agricones. MALDI-MSI confirmed that localization of ginsenosides in the cortex ...

  1. Mass spectrometric investigation of fluorated europium. beta. -diketonates. [Electrons

    Energy Technology Data Exchange (ETDEWEB)

    Khomenko, V.S.; Lozinskij, M.O.; Fialkov, Yu.A.; Rasshinina, T.A.; Suboch, V.P. (AN Belorusskoj SSR, Minsk. Inst. Fiziki; AN Ukrainskoj SSR, Kiev. Inst. Organicheskoj Khimii)

    Ternary complexes of europium with two organic ligands - fluorated ..beta..-diketone and organic base - in the aqueous phase at electron shock are investigated; regroupings that take place in them are established. Mass-spectrometric investigation has shown that complexes with ..beta..-diketones, containing in oxygen atom in a fluorated radical, eliminate stable molecules of difluorophosgen, CoF/sub 2/. For the complexes studied under the above conditions the Co molecule elimination is also typical which is accompanied by the formation of ions with a metal-carbon bond.

  2. Verifiability of Gamma ray Spectrometric results

    International Nuclear Information System (INIS)

    Full text: With the adoption of the EU legislative the introduction of a quality assurance system and application of quality control procedures become mandatory for testing laboratories. The standard describing the requirements for these laboratories is the ISO 17025 standard. Regarding the service to the client the standard requests cooperation in monitoring the laboratory's performance. The client's confidence in measurement results is especially important in measurements of radioactivity since alternative measurement methods can be very expensive. Therefore the concept of verifiability, i.e. the property of the results, which enables the client to assess their reliability, is implemented. Verifiability is implemented by reporting the activity of 40K and the concentration of potassium in the sample. 40K emits gamma rays and its activity in the sample is determined simultaneously with the activities of other photon emitters. Since the isotopic composition of potassium is constant, the activity of 40K is proportional to the concentration of potassium in the sample, which can be measured chemically. In this way we enable the client to assess the reliability of our measurement of 40K by chemical methods. Disagreement in the potassium concentrations results would cause doubts in the reliability of other results obtained by gamma-ray spectrometry and would result in an assessment of the sample preparation and measurement procedure.(author)

  3. Mass spectrometric analysis of monolayer protected nanoparticles

    Science.gov (United States)

    Zhu, Zhengjiang

    Monolayer protected nanoparticles (NPs) include an inorganic core and a monolayer of organic ligands. The wide variety of core materials and the tunable surface monolayers make NPs promising materials for numerous applications. Concerns related to unforeseen human health and environmental impacts of NPs have also been raised. In this thesis, new analytical methods based on mass spectrometry are developed to understand the fate, transport, and biodistributions of NPs in the complex biological systems. A laser desorption/ionization mass spectrometry (LDI-MS) method has been developed to characterize the monolayers on NP surface. LDI-MS allows multiple NPs taken up by cells to be measured and quantified in a multiplexed fashion. The correlations between surface properties of NPs and cellular uptake have also been explored. LDI-MS is further coupled with inductively coupled plasma mass spectrometry (ICP-MS) to quantitatively measure monolayer stability of gold NPs (AuNPs) and quantum dots (QDs), respectively, in live cells. This label-free approach allows correlating monolayer structure and particle size with NP stability in various cellular environments. Finally, uptake, distribution, accumulation, and excretion of NPs in higher order organisms, such as fish and plants, have been investigated to understand the environmental impact of nanomaterials. The results indicate that surface chemistry is a primary determinant. NPs with hydrophilic surfaces are substantially less toxic and present a lower degree of bioaccumulation, making these nanomaterials attractive for sustainable nanotechnology.

  4. Determination of major phenolic acids, phenolic diterpenes and triterpenes in Rosemary (Rosmarinus Officinalis L.) by gas chromatography and mass spectrometry:

    OpenAIRE

    Vončina, Ernest; Doleček, Valter; Islamčević Razboršek, Maša; Brodnjak-Vončina, Darinka

    2007-01-01

    A gas chromatographic-mass spectrometric (GC-MS) method for the simultaneous identification and quantification of seven major phenolic and terpenic compounds in Rosmarinus officinalis L. was developed. The compounds were identified as trimethylsilyl (TMS) derivatives of phenolic acids (caffeic and rosmarinic acid), phenolic diterpene (carnosic acid), and pentacyclic triterpenes (ursolic, oleanolic, betulinic acid and betulin). These compounds have been identified by retention time and compari...

  5. UNTERSUCHUNGEN ZUM NACHWEIS UND ZUR BIOTRANSFORMATION EINIGER ORAL WIRKSAMER 17α-ALKYL-STEROIDE MIT ANABOLER WIRKUNG BEIM PFERD

    OpenAIRE

    Schoene, Claudia

    2010-01-01

    This study tried to investigate the metabolism of the anabolic steroids dehydroepiandrosterone (DHA), methandriol (MAD) and 17α-methyltestosterone (17α-MT) in the Equine and to subsequently develop a gas-chromatographic / mass-spectrometric (gc/ms) screening method for the detection of the two latter orally-active anabolic agents. For each experiment 200 mg of the respective steroid were administered to two thoroughbred horses in training. The administered substances contained a ...

  6. Depth profiling of inhomogeneous zirconia films by optical and Rutherford backscattering spectrometric techniques

    International Nuclear Information System (INIS)

    A method of determining an average refractive-index of a transparent inhomogeneous film on a transparent substrate is proposed. It requires making measurements at normal incidence of the transmittance from the sample using a readily available spectrophotometer. The usefulness of the technique is demonstrated by successful application to thermally evaporated zirconia (ZrO2) samples, a type known to present troublesome examples of optical inhomogeneity. Depth profiles of the zirconia films obtained by optical and Rutherford backscattering spectrometric techniques support an earlier model of an inhomogeneous film with a columnar structure. In that reported model it is suggested that the film retains the hexagonal array of closely packed circular bases of the columns and that the columnar diameters decrease with the distance from the substrate side of the film. (author)

  7. Mass-spectrometric determination of trace elements in aqueous media without preconcentration

    Energy Technology Data Exchange (ETDEWEB)

    Foss, G. O.

    1981-10-01

    Feasibility of using a low pressure glow discharge as an ion source for the mass spectrometric determination of trace elements in aqueous media was investigated. A cryogenically cooled hollow cathode ion source was developed to analyze aqueous samples without external preconcentration. Aqueous solutions containing seventy elements were analyzed and the detection limits, sensitivity factors, and linear regression correlation coefficients were determined. A standard test solution of trace elements in water was analyzed and the concentrations of trace elements were calculated using the sensitivity factors determined previously. The results compared favorably within the error limits predicted by the semiquantitative survey methods used. Tap water and natural lake water samples were examined and minimal interference effects due to organic compounds and biological compounds were noted. A research ion optical system (RIOS) was developed as a flexible mass analyzer for the development of new ion sources. The RIOS is a double focussing mass analyzer designed utilizing the Mattauch-Herzog geometry with externally adjustable slit assemblies.

  8. ESR spectrometric characterization of the methyl viologen dosimeter in poly(vinyl alcohol) film

    Science.gov (United States)

    Nishimoto, Sei-Ichi; Ye, Mu; Lu, Yiqun; Kawamura, Takashi; Kagiya, Tsutomu

    A dosimeter of poly(vinyl alcohol) (PVA) film containing methyl viologen dichloride (MV 2+ (Cl -) 2) was characterized by means of ESR and u.v. spectrometries. γ-irradiation of the MV 2+-PVA dosimeter induced one-electron reduction of MV 2+· to thecation radical (MV +), thus giving rise to blue coloration. The resulting MV +· showed an ESR signal with a g-factor of 2.0031. The yield of MV +· at a given radiation dose was estimated from duplicate integral of the ESR first-derivative spectra by reference to 1,1'-diphenyl-2-picrylhydrazyl (DPPH). The yield of MV +· thus estimated increased linearly with increasing the radiation dose up to about 1.4 Mrad. The ESR spectrometry of MV +· showed a linear correlation with the u.v. spectrometric method reported previously.

  9. Standalone multidetector alpha-spectrometric counting and analysis system

    International Nuclear Information System (INIS)

    This document describes the usage and maintenance of a standalone radioactivity counting and analysis system called LOW LEVEL PHA. It was developed for use in multi-sample alpha spectrometric analysis. The LOW LEVEL PHA system is controlled by a MIK-11/2 microcomputer in 28K of memory and utilizes a double density, dual-floppy disk for data storage. Detectors are interfaced to the computer via CAMAC equipment (Computer Automated Measurement and Control). The system supports 32 simultaneously active and independent alpha particle detectors. It operates with collection rates of up to 300 counts per second from all active detectors, using 128 channels per spectrum and a dynamic energy range of 1.5 MeV. The system is not limited, however, to these conditions. In addition to spectral acquisition, the system provides several analysis functions which include peak identification, curve-smoothing, integration, linear and logarithmic scale graphics, and corrections for base-line shift, deadtime, and background counts. These functions can be implemented while other spectra are being collected. The LOW LEVEL PHA system represents a highly cost-effective means of acquiring alpha spectrometric data from a large number of samples simultaneously, with rapid data analysis capability. This is particularly suitable to analytical and environmental research applications where a small number of alpha-emitting radionuclides are measured at a time, e.g., isotopes of Pu or Am. 23 figures

  10. Mass spectrometric detection of radiocarbon for dating applications

    Energy Technology Data Exchange (ETDEWEB)

    Synal, H.-A., E-mail: synal@phys.ethz.ch [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland); Schulze-Koenig, T.; Seiler, M.; Suter, M.; Wacker, L. [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland)

    2013-01-15

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV {sup 14}C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  11. Analysis of spectrometric optical data from different devices

    Science.gov (United States)

    Borisova, D.; Petkov, D.

    2014-10-01

    Remote sensing is a general tool to investigate the different areas of Earth and planets. The development of the implementation capabilities of the optoelectronic devices which are long-term-tested in the laboratory, in the field and are mounted on-board of the remote sensing platforms further improves the capability of instruments to acquire information about the Earth and its resources in different scales. Remote sensing application in the Earth observation begins with the design and the assembling of equipment for carrying out research of the monitored objects remotely and without disturbing their integrity. Ground-truth data in the Earth observation of the environment and in the remote sensing investigations are very important. Remote sensing methods for studying of rocks and minerals are closely related to current programs for the mineral and chemical composition study of the Earth, Mars and Phobos surfaces. The experience and the knowledge from previous experiments in space missions encourage us to continue our efforts to acquire spectral data using different remote sensing systems and to compare the obtained results. The main goal in the geological remote sensing is the determination of the chemical and/or mineral composition and the structure of the rocks. For this purpose the laboratory and the field spectroscopy measurements are performed. These measurements are made to collect, compile and complete guide with spectral characteristics of different rocks for their reliable identification and for the determination of their mineral and chemical composition. The experiments are based on major physical principles such as light scattering, absorption of light, and reflection of light in the electromagnetic spectrum. For the purpose of present paper ex-situ spectroscopy measurements of the granites and their rock-forming minerals from the territory of Bulgaria in visible and near infrared (VNIR) range of the electromagnetic spectrum were performed using

  12. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  13. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  14. Realisation of a {beta} spectrometer solenoidal and a double {beta} spectrometer at coincidence; Realisation d'un spectrometre {beta} solenoidal et d'un double spectrometre {beta} a coincidence

    Energy Technology Data Exchange (ETDEWEB)

    Moreau, J. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-06-15

    The two spectrometers have been achieved to tackle numerous problems of nuclear spectrometry. They possess different fields of application that complete themselves. The solenoidal spectrometer permits the determination of the energy limits of {beta} spectra and of their shape; it also permits the determination of the coefficients of internal conversion and reports {alpha}{sub K} / {alpha}{sub L} and it is especially efficient for the accurate energy levels of the {gamma} rays by photoelectric effect. The double coincidence spectrometer has been conceived to get a good efficiency in coincidence: indeed, the sum of the solid angles used for the {beta} and {gamma} emission is rather little lower to 4{pi} steradians. To get this efficiency, one should have sacrificed a little the resolution that is lower to the one obtained with the solenoidal spectrometer for a same brightness. Each of the elements of the double spectrometer can also be adapted to the study of angular correlations {beta}{gamma} and e{sup -}{gamma}. In this use, it is superior to the thin magnetic lens used up to here. The double spectrometer also permits the survey of the coincidences e{sup -}e{sup -}, e{sup -}{beta} of a equivalent way to a double lens; it can also be consider some adaptation for the survey of the angular correlations e{sup -}e{sup -}, e{sup -}{beta}. Finally, we applied the methods by simple spectrometry and by coincidence spectrometry, to the study of the radiances of the following radioelements: {sup 76}As (26 h), {sup 122}Sb (2,8 j), {sup 124}Sb (60 j), {sup 125}Sb (2,7 years). (M.B.) [French] Les deux spectrometres qui ont ete realises permettent d'aborder un grand nombre de problemes de spectrometrie nucleaire. Ils possedent des champs d'application tres differents qui se completent. Le spectrometre solenoidal permet la determination des energies limites des spectres {beta} et de leur forme; il permet aussi la determination des coefficients de conversion interne et

  15. Method-MS, final report 2010

    OpenAIRE

    Skipperud, Lindis; Popic, Jelena M.; Roos, Per; Salminen, Susanna; Nygren, Ulrika; Sigmarsson, Olgeir; Palsson, Sigurdur Emil

    2011-01-01

    Radiometric determination methods, such as alpha spectrometry require long counting times when low activities are to be determined. Mass spectrometric techniques as Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Thermal Ionisation Mass Spectrometry (TIMS) and Accelerator Mass Spectrometry (AMS) have shown several advantages compared to traditional methods when measuring long-lived radionuclides. Mass spectrometric methods for determination of very low concentrations of elemental isoto...

  16. A new Approach to estimate Isotopic Ratios in Nuclear and Radiological Materials from Nuclear Spectrometric Measurements with Count Rates Close to Background.

    OpenAIRE

    Steiner, Martin; ZAEHRINGER Matthias; BERLIZOV Andriy; KIRCHNER Gerald

    2009-01-01

    Quantification and interpretation of isotopic ratios is generally acknowledged as a powerful method in nuclear forensic analyses to identify the origin of nuclear and radiological materials or the contamination source of environmental media. Nuclear spectrometric measurements provide a straightforward, relatively easy and fast technique for such analyses, which can even be performed on site for gamma emitting radioisotopes. However, radioisotopes relevant for nuclear forensic analyses ofte...

  17. Characterization of pitofenone by EI mass spectrometry and GC/MS system

    Science.gov (United States)

    Popeneciu, H.; Moldovan, Z.; Ristoiu, D.

    2013-11-01

    Pharmaceutical residues in the environment, and their potential toxic effects, have been recognized as one of the emerging research area in the environmental chemistry. Pitofenone is a drug which has antispasmodic effect. This compound is included in few commercial pharmaceutical products as Spasmalgon, Baralgin, Boralgin or Litorgin and therefore after consume can reach the environment on the way of urban water treatment. For a quantitative determination in environmental matrix the chromatographic and mass spectrometric configuration is need. The paper presents a method based on gas chromatographic-mass spectrometric system for pitofenone determination in water matrix.

  18. Gamma spectrometric system for measuring low and medium radioactive samples

    International Nuclear Information System (INIS)

    Measuring radioactive samples from environment and animal sub-products which usually have low radioactivity and a mixture of a radionuclides, requires the use of complex spectrometric systems. In our Department such a system was development, currently equipped with scintillation detector. All the electronic modules (High Voltage Supply, Pulse Amplifier, ADC) in the system are fully digitally controlled by the computer via a specialized interface and a special device driver, which is a resident program. The spectrum acquisition is performed in the background by the device driver. Spectrum processing (peak search, background subtraction, radionuclide identification, energy and efficiency calibration, activity and associated error calculation) is done by a special application which has a user friendly graphic interface and includes database and reporting facilities. The next year the system will be equipped with an automatic sample changer for large volume samples. We intend to provide the possibility to use also a HPGe detector. (authors)

  19. Quality assurance of automated gamma-ray spectrometric analysis

    International Nuclear Information System (INIS)

    Fully automatic gamma-ray spectrometric analysis procedures perform complete processing of the spectrum without intervention of the operator. In order to maintain the reliability of the final results the analysis checks the intermediate results automatically. When a disagreement is identified by such a check the uncertainty of the intermediate results is increased in order to accommodate the disagreement. The increased uncertainty is propagated into the uncertainty of the final results in order to take into account the disagreement. This approach was implemented in Canberra's Genie ESP gamma-ray spectrometry package for examining the results of the peak analysis. In addition to this intermediate check also a-posteriori checks of the final results can be performed by statistical analysis. Such analysis shows whether the results are under statistical control and can discover sources of variability which are not taken into account in the uncertainty budget

  20. Gamma-spectrometric results concerning campaign 3. DOMO programme

    Energy Technology Data Exchange (ETDEWEB)

    Willekens, V.

    1996-05-01

    The aim of the DOMO programme is to investigate in three successive campaigns the behaviour of Mixed Oxide (MOX) fuel irradiated up to high burn-up. A fuel rod has been irradiated in the Dodewaard reactor at steady state conditions in order to obtain the required burn-up. The irradiated rods were subjected to a power transient in the PWC-CCD capsule. During the irradiation in the PWC-CCD capsule, the rod power was determined by making the thermal balance of the incoming and outgoing cooling water of the loop. For an independent check of the thermal balance, gamma spectrometry on fission products in the rod was performed after-after irradiation. The gamma spectrometric measurements on the segments U10, X42, J06 of the DOMO programme are described. These measurements were set up in order to determine the power and the burn-up of the segments.

  1. Gamma-spectrometric results concerning campaign 3. DOMO programme

    International Nuclear Information System (INIS)

    The aim of the DOMO programme is to investigate in three successive campaigns the behaviour of Mixed Oxide (MOX) fuel irradiated up to high burn-up. A fuel rod has been irradiated in the Dodewaard reactor at steady state conditions in order to obtain the required burn-up. The irradiated rods were subjected to a power transient in the PWC-CCD capsule. During the irradiation in the PWC-CCD capsule, the rod power was determined by making the thermal balance of the incoming and outgoing cooling water of the loop. For an independent check of the thermal balance, gamma spectrometry on fission products in the rod was performed after-after irradiation. The gamma spectrometric measurements on the segments U10, X42, J06 of the DOMO programme are described. These measurements were set up in order to determine the power and the burn-up of the segments

  2. X-ray fluorescence spectrometric and optical emission spectographic analysis of thoria in thoriated copper metal powder

    International Nuclear Information System (INIS)

    Two methods, one using the X-ray fluorescence (XRF) spectrometric technique and another using optical emission spectrographic (OES) technique are described for the determination of thoria in the concentration range 0.5-10% in thoriated copper metal powder. The precision of XRF method is superior to OES method but when sample quantity is very small, the OES method is useful. For XRF method, 500 mg sample is mixed with boric acid binding material and converted to a tablet for analysis. For OES method, only 200 mg sample is needed which is glued to the flat ends of two graphite electrodes for excitation by AC arc. The precision obtained in XRF is better than +-1% and in OES it is +-23%. (author)

  3. Mass spectrometric determination of early and advanced glycation in biology.

    Science.gov (United States)

    Rabbani, Naila; Ashour, Amal; Thornalley, Paul J

    2016-08-01

    Protein glycation in biological systems occurs predominantly on lysine, arginine and N-terminal residues of proteins. Major quantitative glycation adducts are found at mean extents of modification of 1-5 mol percent of proteins. These are glucose-derived fructosamine on lysine and N-terminal residues of proteins, methylglyoxal-derived hydroimidazolone on arginine residues and N(ε)-carboxymethyl-lysine residues mainly formed by the oxidative degradation of fructosamine. Total glycation adducts of different types are quantified by stable isotopic dilution analysis liquid chromatography-tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring mode. Metabolism of glycated proteins is followed by LC-MS/MS of glycation free adducts as minor components of the amino acid metabolome. Glycated proteins and sites of modification within them - amino acid residues modified by the glycating agent moiety - are identified and quantified by label-free and stable isotope labelling with amino acids in cell culture (SILAC) high resolution mass spectrometry. Sites of glycation by glucose and methylglyoxal in selected proteins are listed. Key issues in applying proteomics techniques to analysis of glycated proteins are: (i) avoiding compromise of analysis by formation, loss and relocation of glycation adducts in pre-analytic processing; (ii) specificity of immunoaffinity enrichment procedures, (iii) maximizing protein sequence coverage in mass spectrometric analysis for detection of glycation sites, and (iv) development of bioinformatics tools for prediction of protein glycation sites. Protein glycation studies have important applications in biology, ageing and translational medicine - particularly on studies of obesity, diabetes, cardiovascular disease, renal failure, neurological disorders and cancer. Mass spectrometric analysis of glycated proteins has yet to find widespread use clinically. Future use in health screening, disease diagnosis and therapeutic monitoring, and

  4. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  5. Mass spectrometric characterization of the rubber elongation factor - major allergen in natural latex gloves

    International Nuclear Information System (INIS)

    The aim of the present work is the mass spectrometric characterization of the possible latex allergens present in natural latex gloves. The introduction covers a brief description of the molecular basis and types of allergens, and some of the promising therapeutic possibilities. It shows the composition of the natural latex milk and gives a summary of the conversion of the raw material into its products. The most important natural latex allergens are described and the knowledge about the medical aspects of this illness are summarized. The different chemical and biological methods applied during this study are also introduced in this chapter from the simple methods for protein extraction to the sophisticated ones for primary structure characterization. Chapter 4.1. describes the mass spectrometric analysis of the natural latex milk. Different samples - representing subsequent steps of processing of the raw material before the production of the gloves - were investigated. The effects of the sample preparation methods on the MALDI MS measurements were studied and compared. Several compounds could be detected in the freshly tapped natural latex sap and the change of the composition of the milk following the steps of preparation could be observed. Natural latex gloves were investigated in chapter 4.2. without extraction, directly by means of MALDI mass spectrometry. The protein pattern of the gloves during production - before and after the washing steps - was investigated. We found not only a difference between these two stages of the process, but also a variation of the protein pattern on the inner and outer sides of the gloves. Several types of finished products were studied and it could be concluded, that the detection of a part of the proteins revealed in the natural latex milk is still possible in this goods with MALDI mass spectrometry, without extraction and purification. It turned out, that the characteristics of the surface and the pore structure of the gloves

  6. Molecular assessment of surgical-resection margins of gastric cancer by mass-spectrometric imaging.

    Science.gov (United States)

    Eberlin, Livia S; Tibshirani, Robert J; Zhang, Jialing; Longacre, Teri A; Berry, Gerald J; Bingham, David B; Norton, Jeffrey A; Zare, Richard N; Poultsides, George A

    2014-02-18

    Surgical resection is the main curative option for gastrointestinal cancers. The extent of cancer resection is commonly assessed during surgery by pathologic evaluation of (frozen sections of) the tissue at the resected specimen margin(s) to verify whether cancer is present. We compare this method to an alternative procedure, desorption electrospray ionization mass spectrometric imaging (DESI-MSI), for 62 banked human cancerous and normal gastric-tissue samples. In DESI-MSI, microdroplets strike the tissue sample, the resulting splash enters a mass spectrometer, and a statistical analysis, here, the Lasso method (which stands for least absolute shrinkage and selection operator and which is a multiclass logistic regression with L1 penalty), is applied to classify tissues based on the molecular information obtained directly from DESI-MSI. The methodology developed with 28 frozen training samples of clear histopathologic diagnosis showed an overall accuracy value of 98% for the 12,480 pixels evaluated in cross-validation (CV), and 97% when a completely independent set of samples was tested. By applying an additional spatial smoothing technique, the accuracy for both CV and the independent set of samples was 99% compared with histological diagnoses. To test our method for clinical use, we applied it to a total of 21 tissue-margin samples prospectively obtained from nine gastric-cancer patients. The results obtained suggest that DESI-MSI/Lasso may be valuable for routine intraoperative assessment of the specimen margins during gastric-cancer surgery. PMID:24550265

  7. Lipopeptides from the Banyan Endophyte, Bacillus subtilis K1: Mass Spectrometric Characterization of a Library of Fengycins

    Science.gov (United States)

    Pathak, Khyati V.; Keharia, Haresh; Gupta, Kallol; Thakur, Suman S.; Balaram, Padmanabhan

    2012-10-01

    Mass spectrometric analysis of a banyan endophyte, Bacillus subtilis K1, extract showing broad spectrum antifungal activity revealed a complex mixture of lipopeptides, iturins, surfactins, and fengycins. Fractionation by reversed-phase high performance liquid chromatography (HPLC) facilitated a detailed analysis of fengycin microheterogeneity. Matrix assisted laser desorption ionization (MALDI) and electrospray ionization (ESI) mass spectrometric studies permitted the identification of several new fengycin variants. Four major sites of heterogeneity are identified: (1) N-terminus β-hydroxy fatty acid moiety, where chain length variation and the presence of unsaturation occur, (2) position 6 (Ala/Val/Ile/Leu), (3) position 10 (Val/Ile) within the macrocyclic ring, and (4) Gln to Glu replacement at position 8, resulting in fengycin variants that differ in mass by 1 Da. Diagnostic fragment ions provide a quick method for localizing the sites of variation in the macrocycle or the linear segment. Subsequent establishment of the sequences is achieved by MS/MS analysis of linear fengycin species produced by hydrolysis of the macrocyclic lactone. Unsaturation in the fatty acid chain and the presence of linear precursors in the B. subtilis K1 extract are also established by mass spectrometry. The anomalous distribution of intensities within isotopic multiplets is a diagnostic for Gln/Glu replacements. High resolution mass spectrometry facilitates the identification of fengycin species differing by 1 Da by localizing the variable position (Gln8/Glu8) in the fengycin variants.

  8. Systematic development of an enzymatic phosphorylation assay compatible with mass spectrometric detection.

    Science.gov (United States)

    de Boer, A R; Letzel, T; Lingeman, H; Irth, H

    2005-02-01

    The enzymatic peptide phosphorylation by cAMP-dependent protein kinase A (PKA) was optimized and monitored by means of electrospray ionization mass spectrometry (ESI-MS). The direct detection of phosphorylated peptides by MS renders labeling unnecessary, reduces time and labor, due to less initial sample pretreatment. In this study the phosphorylation of the peptide malantide by PKA was performed in batch and reaction compounds were detected by ESI-MS after the incubation time. The subsequent product quantitation was accomplished by using one-point normalization. Applying this set-up, optimum solvent conditions (such as salt and modifier content), concentrations of essential reaction compounds (such as cAMP, Mg2+ and ATP), and the influence of reaction properties (such as pH and reaction time) were determined. The reaction milieu has to be suitable for both, the enzymatic reaction and the mass spectrometric detection. We found that the modifier content and the pH value had to be changed after the enzymatic reaction occurred. Through the addition of methanol and acetic acid, the reaction stopped immediately and a more sensitive mass spectrometric detection could be obtained simultaneously. Furthermore, an inhibitor study was performed, testing the inhibition potency of three protein kinase A inhibitors (PKIs). IC50 values were determined and used to calculate the Ki values, that were 7.4, 19.0 and 340.0 nmol/L for PKI(6-22)amide, PKI(5-24)amide, and PKI(14-24)amide, respectively. These data vary between factor 4.4 (for PKI(6-22)amide) and 8.3 (for PKI(5-24)amide) compared to the Ki values described in literature. However, the Ki values are in good agreement with the data mainly obtained by fluorescence- or radioactivity-based methods. Nevertheless, our results indicate that ESI-MS is a realistic alternative to radioactivity and fluorescence detection in determining enzymatic activity. Furthermore we were able to illustrate its high potential as a quantitative

  9. Mass spectrometric detection of proteins in non-aqueous media : the case of prion proteins in biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Douma, M.D.; Kerr, G.M.; Brown, R.S.; Keller, B.O.; Oleschuk, R.D. [Queen' s Univ., Kingston, ON (Canada). Dept. of Chemistry

    2008-08-15

    This paper presented a filtration method for detecting protein traces in non-aqueous media. The extraction technique used a mixture of acetonitrile, non-ionic detergent and water along with filter disks with embedded C{sub 8}-modified silica particles to capture the proteins from non-aqueous samples. The extraction process was then followed by an elution of the protein from the filter disk and direct mass spectrometric detection and tryptic digestion with peptide mapping and MS/MS fragmentation of protein-specific peptides. The method was used to detect prion proteins in spiked biodiesel samples. A tryptic peptide with the sequence YGQGSPGGNR was used for unambiguous identification. Results of the study showed that the method is suitable for the large-scale testing of protein impurities in tallow-based biodiesel production processes. 33 refs., 6 figs.

  10. Separation of trace antimony and arsenic prior to hydride generation atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    A separation method utilizing a synthetic zeolite (mordenite) was developed in order to eliminate the gas phase interference of Sb(III) on As(III) during quartz furnace hydride generation atomic absorption spectrometric (HGAAS) determination. The efficiency of the proposed separation method in the reduction of suppression effects of transition metal ions on As(III) signal was also investigated. Among the volatile hydride-forming elements and their different oxidation states tested (Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), and Te(VI)), only Sb(III) was found to have a signal depression effect even at low (μg l-1) concentrations under the experimental conditions employed. It has been shown that mordenite adsorbs Sb(III) quantitatively, even at a concentration of 1000 μg l-1, at pHs greater than two, and also, it reduces the initial concentrations of the transition metal ions to lower levels which can be tolerated in many studies. The adsorption of Sb(III) on mordenite follows the Freundlich isotherm and is endothermic in nature

  11. Targeted selected reaction monitoring mass spectrometric immunoassay for insulin-like growth factor 1.

    Directory of Open Access Journals (Sweden)

    Eric E Niederkofler

    Full Text Available Insulin-like growth factor 1 (IGF1 is an important biomarker of human growth disorders that is routinely analyzed in clinical laboratories. Mass spectrometry-based workflows offer a viable alternative to standard IGF1 immunoassays, which utilize various pre-analytical preparation strategies. In this work we developed an assay that incorporates a novel sample preparation method for dissociating IGF1 from its binding proteins. The workflow also includes an immunoaffinity step using antibody-derivatized pipette tips, followed by elution, trypsin digestion, and LC-MS/MS separation and detection of the signature peptides in a selected reaction monitoring (SRM mode. The resulting quantitative mass spectrometric immunoassay (MSIA exhibited good linearity in the range of 1 to 1,500 ng/mL IGF1, intra- and inter-assay precision with CVs of less than 10%, and lowest limits of detection of 1 ng/mL. The linearity and recovery characteristics of the assay were also established, and the new method compared to a commercially available immunoassay using a large cohort of human serum samples. The IGF1 SRM MSIA is well suited for use in clinical laboratories.

  12. Determination of ash content of coal using nuclear borehole logging spectrometric gamma-gamma technique

    International Nuclear Information System (INIS)

    During the past decade, increasing effort has been given to monitoring coal quality in the search, production and preparation sequence. Considerable research and development has been carried out on nuclear methods for determination of ash in coal. A number of nuclear techniques are now well established for coal analysis. In particular, the spectrometric gamma-gamma technique is based on the existence of a simple correlation between the ash content and the equivalent atomic number of coal. This technique records and uses the count rates of the backscatter spectrum. These count rates describe the changes in spectral shape which are due to ash content variations. This method is presented along with a short review of the physical background. The report includes the simulation of in situ borehole probe readings using a MONTE CARLO tracking program. Simulating the transport through matter of gamma-rays by MONTE CARLO techniques essentially attempts to reproduce the actual statistical nature of the interaction processes. Random numbers are used throughout, along with known nuclear data, to select the parameters which influence a particle's history. Such an approach can deal with complex geometries through which the particles move. Biaising or weightening techniques are applied for variance reduction, so as to minimise the statistical errors. The basic features of biaising as well as the description of the program are given. A semi-theoretical approach is discussed for the determination of ash content of coal seam using the simulated spectrum

  13. Mass spectrometric study of the amipurimycin hexopyranosidic sugar moiety

    Science.gov (United States)

    Almoster Ferreira, M. A.; Borges, C.; Oliveira, M. C.; Pocsfalvi, G.; Rauter, A. P.; Fernandes, A. C.

    1997-11-01

    Amipurimycin is a natural nucleoside that displays a remarkable activity in vitro and in vivo against Pyricularia oryzae, which is responsible for the rice blast disease. Six important precursors for the synthesis of the Amipurimycin sugar moiety were prepared. In order to obtain structural information a mass spectrometric study of these compounds was performed using liquid secondary ion mass spectrometry (LSIMS) with high-energy collision-induced dissociation (CID) experiments on a four-sector instrument. Elimination of methanol is the preferential fragmentation path for five of the six protonated molecules, indicating that protonation plays an important role in the process, whilst for the other protonated molecule loss of water is the main fragmentation. Examination of the [M + Li]+ precursor ion spectra shows that loss of methanol does not occur in three of them, but in the other three gives rise to fairly abundant ions, indicating that in this case methanol elimination implies intramolecular hydrogen transfer, the resulting ion having a very stable structure.

  14. Deep UV imaging by spectrometric full-colour cathodoluminescence microscopy

    International Nuclear Information System (INIS)

    A new deep-UV cathodoluminescence (CL) microscopy is tried on studying design and fabrication of recent solid-state light-emitting (LE) devices that emit near 200 nm light. CL microscopy has enough energy for electronic excitation of deep-UV emitting devices and visualizes distribution map of their electronic structures. The deep-UV imaging system is constructed on our own spectrometric full-colour CL microscope that collects CL spectra at all pixel points of the specimen during regular SEM observation, and at the end of one frame scan, a set of CL spectra is accumulated in the control computer. One frame scan of 512x512 pixels needs 8 to 80 sec, which is unbeatable by any other commercial CL microscopes. Full-colour CL micrograph is constructed using the spectra. The detector, a 32-channel photoelectron multiplier array, has higher sensitivity in UV region than any solidstate linear sensors, and a grating of 300-nm blaze wavelength instead of one at 500-nm blaze wavelength for visible lights, provide CL micrographs of 180-700 nm lights for recent deep-UV LE devices. Some unforeseen light emissions between 200-350 nm regions are observed on various materials and they are discussed correlating with the structure observed in SEM micrographs.

  15. Radio spectrometric survey of un-surveyed areas in Syria

    International Nuclear Information System (INIS)

    The values and distribution of the radioelements e U, e Th, % K and Ur units in the surface geological formations of the west and south sectors of Syrian region, were estimated using carbone gamma ray spectrometric survey. The radiometric maps were prepared, as well as, many geological profiles, cross sections studied in different locations and geochemical samples were analyzed by laboratory gamma ray spectrometry and by x-ray diffractometry, the results of the all sets were compared. In general, the survey shows, low radioelement concentrations in the area, especially on basic rocks (Jabal Al-arab, Hawran) south Syria, and on ultra basic rocks (ophiolitic complex) north-west Syria, but there are some separate anomalous spots were connected with phosphate rocks, detected on cretaceous and Palaeogene age. Some times we noticed high radioelement concentrations haloes associated with fractured zones were already arise from secondary uranium mineralization, as a result of solutions movement through fissures in carbonatic and/or chalk like limestone rocks. finally, the obtained concentrations, represent a background values which has no significant importance for uranium exploration point of view. (author)

  16. Functional proteomics with new mass spectrometric and bioinformatics tools

    International Nuclear Information System (INIS)

    A comprehensive range of mass spectrometric tools is required to investigate todays life science applications and a strong focus is on addressing the needs of functional proteomics. Application examples are given showing the streamlined process of protein identification from low femtomole amounts of digests. Sample preparation is achieved with a convertible robot for automated 2D gel picking, and MALDI target dispensing. MALDI-TOF or ESI-MS subsequent to enzymatic digestion. A choice of mass spectrometers including Q-q-TOF with multipass capability, MALDI-MS/MS with unsegmented PSD, Ion Trap and FT-MS are discussed for their respective strengths and applications. Bioinformatics software that allows both database work and novel peptide mass spectra interpretation is reviewed. The automated database searching uses either entire digest LC-MSn ESI Ion Trap data or MALDI MS and MS/MS spectra. It is shown how post translational modifications are interactively uncovered and de-novo sequencing of peptides is facilitated

  17. Mass spectrometric searches for superheavy elements in terrestrial matter

    Science.gov (United States)

    Korschinek, Gunther; Kutschera, Walter

    2015-12-01

    Recent searches for traces of long-lived superheavy elements (SHEs) in terrestrial materials by mass spectrometric means are reviewed. Positive evidence for long-lived neutron-deficient Th isotopes in Th and Rg isotopes in Au, and a possible A = 292, Z ∼ 122 nuclide in Th was reported from experiments with Inductively Coupled Plasma Sector Field Mass Spectrometry (ICP-SF-MS). These findings were not confirmed with Accelerator Mass Spectrometry (AMS), with abundance limits lower by several orders of magnitude. In addition, the extensive AMS searches for 42 SHE nuclides (A = 288- 310) around the much discussed "island of stability" (Z = 114, N = 184) in natural Pt, Au, Pb, Bi materials are reviewed. Due to the flatness of the mass distribution and the relatively large bandwidth of the mass acceptance in AMS searches, an effectively much larger number of SHE nuclides was scanned in the respective materials. No positive evidence for the existence of long-lived SHEs (t1/2 >108 yr) with abundance limits of 10-12 to 10-16 was found.

  18. QuEChERS: um método moderno de preparo de amostra para determinação multirresíduo de pesticidas em alimentos por métodos cromatográficos acoplados à espectrometria de massas QuEChERS: a modern sample preparation method for pesticide multiresidue determination in food by chromatographic methods coupled to mass spectrometry

    Directory of Open Access Journals (Sweden)

    Osmar D. Prestes

    2009-01-01

    Full Text Available This review attempts to provide an updated overview of the Quick, Easy, Cheap, Effective, Ruged and Safe (QuEChERS multiresidue extraction method, that involves initial extraction in acetonitrile, an extraction/partition step after the addition of salt, and a cleanup step utilizing dispersive solid phase extraction. QuEChERS method is nowadays the most applied extraction method for the determination of pesticide residues in food samples, providing acceptable recoveries for acidic, neutral and basic pesticides. Several applications for various food matrices (fruits, vegetables, cereals and others in combination with chromatographic mass spectrometry analysis were presented.

  19. Some applications of spectrometric gamma-ray logging in prospecting of oil and hard-coal deposits

    International Nuclear Information System (INIS)

    The paper presents the results of application of gamma-ray spectrometric method in the oil, gas and hard-coal prospecting. The use of bore hole spectrometer made possible to determine in situ concentrations of natural radioisotopes: K, U and Th. The knowledge of K, U and Th concentrations gives a mineralogic information which combined with other geophysical parameters such as; density, Pe and neutron porosity constitutes a valuable tool for prospection of the investigated layers. The presented anomalies of uranium concentrations can be important in the determination of shale concentration in the rocks. The method when applied in a hard coal deposit made possible to identify the coal seams and their thickness. The determined concentrations of U, Th and K were used to calculate the calorific value, ash content and carbon-element content in the coal. (author)

  20. Development of a mass spectrometrical isotope dilution analysis for determination of trace iodine levels and its application for food samples

    International Nuclear Information System (INIS)

    A mass spectrometrical isotope dilution procedure for the determination of trace amounts of iodine in various materials was developed using 129I as indicator isotope, based on the determination of the 129I/127I isotope relationship. Negative thermionization was used as ionization method. The analysis procedure, which worked with a standard deviation of between 0,1 and 10% (depending on material tested), was used to determine the iodine level of table salt - both iodized and normal salt (3-6 ppm and less than 0,006 ppm respectively), and food samples with an organic matrix. For comparison the iodine levels were also measured with an iodine-selective electrode. Special preparation and separation procedures were done to suit the sample material. A comparison of the levels of iodine concentration in various powdered milks which were measured by international collaborators using varying methods shows the superior reproducibility of the MS-IDA. (RB)

  1. Mass spectrometric behaviour of carboxylated polyethylene glycols and carboxylated octylphenol ethoxylates.

    Science.gov (United States)

    Frańska, Magdalena; Zgoła, Agnieszka; Rychłowska, Joanna; Szymański, Andrzej; Łukaszewski, Zenon; Frański, Rafał

    2003-01-01

    Mass spectrometric behaviour of mono- and di-carboxylated polyethylene glycols (PEGCs and CPEGCs) and carboxylated octylphenol ethoxylates (OPECs) are discussed. The tendency for ionisation (deprotonation, protonation and cationisation by alkali metal cations) of carboxylated PEGs was compared with that of non-carboxylated correspondents by using both secondary ion mass spectrometry (SIMS) and electrospray ionisation (ESI). The fragmentation of the PEGCs and CPEGCs is discussed and also compared with their neutral correspondents, PEGs. The B/E mass spectra were recorded, using secondary ion mass spectrometry as a method for generation, for deprotonated and protonated molecules and molecules cationised by alkali metal cations. The fragmentation behaviour of PEGs is found to be different from that of CPEGCs, The presence of carboxylic groups may be confirmed not only by the determination of molecular weights of the ethoxylates studied, but also on the basis of the fragment ions formed. The metastable decomposition of the [OPEC-H](-) ions proceed through the cleavage of the bond between the octylphenol moiety and the ethoxylene chain leading to the octylphenoxy anions. It permits determination of the mass of the hydrophobic moiety of the studied carboxylated alkylphenol ethoxylate. ESI mass spectra recorded in the negative ion mode were found to be more suitable for the determination of the average molecular weight of carboxylated ethoxylates than SI mass spectra. PMID:12939494

  2. Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques.

    Science.gov (United States)

    Lavilla, I; Cabaleiro, N; Costas, M; de la Calle, I; Bendicho, C

    2009-11-15

    In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS+3% (v/v) of HNO(3) or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases. PMID:19782199

  3. Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

    Science.gov (United States)

    Bibi, Aisha; Ju, Huangxian

    2016-04-01

    A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27041659

  4. Advances in mass spectrometric characterization of naphthenic acids fraction compounds in oil sands environmental samples and crude oil--A review.

    Science.gov (United States)

    Headley, John V; Peru, Kerry M; Barrow, Mark P

    2016-01-01

    There has been a recent surge in the development of mass spectrometric methods for detailed characterization of naphthenic acid fraction compounds (all C(c)H(h)N(n)O(o)S(s), species, including heteroatomic and aromatic components in the acid-extractable fraction) in environmental samples. This surge is driven by the increased activity in oil sands environmental monitoring programs in Canada, the exponential increase in research studies on the isolation and toxicity identification of components in oil sands process water (OSPW), and the analytical requirements for development of technologies for treatment of OSPW. There has been additional impetus due to the parallel studies to control corrosion from naphthenic acids during the mining and refining of heavy bitumen and crude oils. As a result, a range of new mass spectrometry tools have been introduced since our last major review of this topic in 2009. Of particular significance are the developments of combined mass spectrometric methods that incorporate technologies such as gas chromatography, liquid chromatography, and ion mobility. There has been additional progress with respect to improved visualization methods for petroleomics and oil sands environmental forensics. For comprehensive coverage and more reliable characterization of samples, an approach based on multiple-methods that employ two or more ionization modes is recommended. On-line or off-line fractionation of isolated extracts, with or without derivatization, might also be used prior to mass spectrometric analyses. Individual ionization methods have their associated strengths and weaknesses, including biases, and thus dependence upon a single ionization method is potentially misleading. There is also a growing trend to not rely solely on low-resolution mass spectrometric methods (power at m/z 200) for characterization of complex samples. Future research is anticipated to focus upon (i) structural elucidation of components to determine the correlation

  5. High-precision mass spectrometric hydrogen isotope ratio measurements

    International Nuclear Information System (INIS)

    The analytical capabilities of mass spectrometric ion-current measurement systems are described on both a theoretical and a practical basis. From the theoretical standpoint, a signal-to-noise ratio (S/N) model that evaluated the fundamental sources of noise present in ion-current measurement systems was developed. Use of this model accurately predicted the performance (precision) for ion-current ratio measurements made by two isotope ratio mass spectrometers, one designed for carbon isotopic measurements, and the other designed for hydrogen isotopic measurements. Isotope ratio measurements differ from current-ratio measurements in that the observed ion-current ratio must be corrected to reflect the ratio of the ion currents due to the isotopic species of interest, which, for hydrogen isotope ratio mass spectrometry, are HD+ and H2+. Interfaces to these two ion currents are described in detail. To compensate for H3+ three measurement procedures, the two-standard calibration, the one-standard differential measurement with electronic H3+ compensation, and the two-standard differential measurement, are described. The one- and two-standard differential measurements were successfully used for measurement of isotopic abundances. Results of a collaborative investigation to validate the use of 18O in place of D as an isotopic label for total body water measurements are presented. In this research both 18O and D were administered simultaneously to several subjects. The weight of total body water of these subjects as measured by the dilution of D into the body water was in good agreement with the results of the 18O measurements. A brief description of the laboratory computer system is also given

  6. Experimental characterization of the Clear-PEM scanner spectrometric performance

    Science.gov (United States)

    Bugalho, R.; Carriço, B.; Ferreira, C. S.; Frade, M.; Ferreira, M.; Moura, R.; Ortigão, C.; Pinheiro, J. F.; Rodrigues, P.; Rolo, I.; Silva, J. C.; Trindade, A.; Varela, J.

    2009-10-01

    In the framework of the Clear-PEM project for the construction of a high-resolution and high-specificity scanner for breast cancer imaging, a Positron Emission Mammography tomograph has been developed and installed at the Instituto Português de Oncologia do Porto hospital. The Clear-PEM scanner is mainly composed by two planar detector heads attached to a robotic arm, trigger/data acquisition electronics system and computing servers. The detector heads hold crystal matrices built from 2 × 2 × 20 mm3 LYSO:Ce crystals readout by Hamamatsu S8550 APD arrays. The APDs are optically coupled to both ends of the 6144 crystals in order to extract the DOI information for each detected event. Each one of 12288 APD's pixels is read and controlled by Application Specific Integrated Circuits water-cooled by an external cooling unit. The Clear-PEM frontend boards innovative design results in a unprecedented integration of the crystal matrices, APDs and ASICs, making Clear-PEM the PET scanner with the highest number of APD pixels ever integrated so far. In this paper, the scanner's main technical characteristics, calibration strategies and the first spectrometric performance evaluation in a clinical environment are presented. The first commissioning results show 99.7% active channels, which, after calibration, have inter-pixel and absolute gain distributions with dispersions of, respectively, 12.2% and 15.3%, demonstrating that despite the large number of channels, the system is uniform. The mean energy resolution at 511 keV is of 15.9%, with a 8.8% dispersion, and the mean CDOI-1 is 5.9%/mm, with a 7.8% dispersion. The coincidence time resolution, at 511 keV, for a energy window between 400 and 600 keV, is 5.2 ns FWHM.

  7. Application and evaluation of the mass spectrometric isotope dilution technique in the determination of rare earths in geological materials

    International Nuclear Information System (INIS)

    Establishment of the experimental procedures employed in the rare earth element determination of geological samples by mass spectrometric isotope dilution analysis is discussed in the present work. The procedures involve preparation and calibration of the isotope tracers isotope dilution, dissolution in a teflon pressure vessel, chemical separation and isotope analysis using a fully automated Micromass VG ISOTOPES model 354 thermal ionization mass spectrometer. For the initial chemical separation of total rare earths the cationic resin was employed and HC1 and HNO3 acids as eluents. In the second step rare earths elements were separated into individual (La, Ce and Nd) and subgroups (Sm-Eu-Gd, Yb-Er-Dy) fractions using the same cationic resin and α-HIBA as eluent. Nine elements La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb are determined by this method in the ''United States Geological Survey'' (USGS) standard samples GSP-1, AGV-1 and G-2, with an overall precision of +- 1 to 2% and an accuracy of 5%. The concentration of rare earth element determined in the standard sample PCC-1 showed that the total analytical blanks are in submicrogram levels. The concentration of rare earth elements in the same USGS standard samples were also determined by Instrumental neutron activation analysis, neutron activation analysis with chemical separation before irradiation and inductively coupled argon plasma spectroscopy. The chemical procedures employed for these methods are the same as that used for mass spectrometric isotope dilution. Based on the results obtained, each method was evaluated pointing out their merits and defects. The study clearly showed that the chemical procedure employed for all these techniques was satisfactory. (author)

  8. Significance of Airborne Gamma-ray spectrometric data of Umm bisilla Area, central Eastern Desert, Egypt

    International Nuclear Information System (INIS)

    Umm bisilla area, located in the Central Eastern Desert of Egypt, consists mainly of basement rocks. The present investigation of the airborne spectrometric data is to define the meaningful anomalies from the raw data by applying the significance factor techniques, by calculating the significant radioactive provinces. Determination of the gross structural pattern and broad variations in composition of the crystalline basement, to define the relationships between the tectonic features of the area as interpreted from aeromagnetic data, with the significant anomalies revealed from spectrometric data was carried out through the application of different magnetic techniques. Five significant uraniferous zones were detected associated with Umm Bisilla granite, amphibolite, and grey granite. The intersection of the structural lineaments interpreted from aeromagnetic data illustrated good correlation with the significant uranium anomalous zones interpreted from spectrometric data, and indicated that the concentration is structurally. 15 figs

  9. Mass-spectrometric monitoring of the intravenous anesthetic concentration in the breathing circuit of an anesthesia machine

    Science.gov (United States)

    Elizarov, A. Yu.; Levshankov, A. I.

    2011-04-01

    Interaction between inhalational anesthetic sevoflurane and an absorber of CO2 (soda lime) in the breathing circuit of an anesthesia machine during low-flow anesthesia (0.5 l of a fresh gaseous mixture per minute) is studied with the mass-spectrometric method. Monitoring data for the concentration of sevoflurane and three toxic products of sevoflurane decompositions (substances A, B, and C) during anesthesia in the inspiration-expiration regime are presented. The highest concentration of substance A is found to be 65 ppm. The biochemical blood analysis before and after anesthesia shows that nephropathy is related to the function of liver toxicity. It is found that inhalational anesthetic sevoflurane influences the concentration of intravenous hypnotic propofol in blood.

  10. Vitamin D-metabolites from human plasma and mass spectrometric analysis by fast heavy ion induced desorption

    International Nuclear Information System (INIS)

    D-vitamin metabolites have been isolated from human serum employing chromatographic techniques. The serum carrier protein for vitamin D (DBP) was first isolated by immunosorbent chromatography. Lipid ligands associated with DBP were then extracted with hexane and separated by high pressure liquid chromatography (HPLC). Detection of vitamin D metabolites by their absorbance of ultraviolet light is not sufficiently sensitive to monitor all vitamin D derivatives from a few millilitres of serum. Therefore, further analyses are necessary to quantitative these compounds. We have begun to develop a mass spectrometric method to achieve a reliable, quantitative procedure. As a first step towards this goal a number of pure samples of vitamin D compounds have been studied in a time-of-flight mass spectrometer based on fast heavy ion induced desorption. All vitamin D compounds examined could be detected and identified by their molecular ion and fragment spectra. (orig.)

  11. A microchip electrophoresis-mass spectrometric platform with double cell lysis nano-electrodes for automated single cell analysis.

    Science.gov (United States)

    Li, Xiangtang; Zhao, Shulin; Hu, Hankun; Liu, Yi-Ming

    2016-06-17

    Capillary electrophoresis-based single cell analysis has become an essential approach in researches at the cellular level. However, automation of single cell analysis has been a challenge due to the difficulty to control the number of cells injected and the irreproducibility associated with cell aggregation. Herein we report the development of a new microfluidic platform deploying the double nano-electrode cell lysis technique for automated analysis of single cells with mass spectrometric detection. The proposed microfluidic chip features integration of a cell-sized high voltage zone for quick single cell lysis, a microfluidic channel for electrophoretic separation, and a nanoelectrospray emitter for ionization in MS detection. Built upon this platform, a microchip electrophoresis-mass spectrometric method (MCE-MS) has been developed for automated single cell analysis. In the method, cell introduction, cell lysis, and MCE-MS separation are computer controlled and integrated as a cycle into consecutive assays. Analysis of large numbers of individual PC-12 neuronal cells (both intact and exposed to 25mM KCl) was carried out to determine intracellular levels of dopamine (DA) and glutamic acid (Glu). It was found that DA content in PC-12 cells was higher than Glu content, and both varied from cell to cell. The ratio of intracellular DA to Glu was 4.20±0.8 (n=150). Interestingly, the ratio drastically decreased to 0.38±0.20 (n=150) after the cells are exposed to 25mM KCl for 8min, suggesting the cells released DA promptly and heavily while they released Glu at a much slower pace in response to KCl-induced depolarization. These results indicate that the proposed MCE-MS analytical platform may have a great potential in researches at the cellular level. PMID:27207575

  12. Metabolism of boldione in humans by mass spectrometric techniques: detection of pseudoendogenous metabolites.

    Science.gov (United States)

    de la Torre, Xavier; Curcio, Davide; Colamonici, Cristiana; Molaioni, Francesco; Botrè, Francesco

    2013-01-01

    Boldione is an anabolic androgenic steroid (AAS) related to boldenone, androstenedione, and testosterone bearing two double bonds in C1 and C4 positions. Boldione is rapidly transformed to the well-known AAS boldenone, being both compounds included in the list of prohibited substances and methods published yearly by the World Anti-Doping Agency (WADA). After the administration of boldione to a male volunteer, the already described urinary metabolites of boldenone produced after reduction in C4, oxydoreduction in C3 and C17, and hydroxylation have been detected. In addition, minor new metabolites have been detected and their structure postulated after mass spectrometric analyses. Finally, the reduction of the double bound in C1 produces metabolites identical to the endogenously produced ones. A method based on gas chromatography coupled to isotope ratio mass spectrometry (GC/C/IRMS) after a urine sample purification by high performance liquid chromatography (HPLC) permitted to confirm the main synthetic like boldione/boldenone metabolite (17β-hydroxy-5β-androst-1-en-3-one) and boldenone at trace levels (synthetic or endogenous origin, and to determine the exogenous origin of metabolites with the same chemical structure of the endogenous ones. The detection of pseudoendogenous androgens of synthetic origin partially overlapped boldenone and its main metabolite detection, being an additional proof of synthetic steroids misuse. By the use of IRMS, the correct evaluation of the modifications of the steroid profile after the administration of synthetic AAS that could be converted into endogenous like ones is possible. PMID:24259377

  13. QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods

    Science.gov (United States)

    This chapter describes an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in foods using gas and/or liquid chromatographic (GC and/or LC) analytical separation and mass spectrometric (MS) detection. The approach is known as QuEChERS, which stands fo...

  14. Thermal ionization mass spectrometric study of U-Pu-O system

    International Nuclear Information System (INIS)

    First inference from a thermal ionization mass spectrometric study of samples corresponding to the ternary U-Pu-O system, especially if high surface ionization temperatures are employed, is likely to be at variance with that from equilibrium vaporization thermodynamic studies, that the atomic species U and Pu dominate the vapor phase

  15. Solid-state UV-MALDI mass spectrometric quantitation of fluroxypyr and triclopyr in soil.

    Science.gov (United States)

    Ivanova, Bojidarka; Spiteller, Michael

    2015-06-01

    The work presented here refers firstly to solid-state UV-MALDI-Orbitrap-mass spectrometric analysis of fluroxypyr (A) and triclopyr (B) in soils under laboratory conditions. The experimental design has involved the following: (a) determination of analytes A and B in polycrystalline composites of organic materials 1-7, based on 2-piperidine (pyrrolidine or piperazine)-1-yl-ethyl ammonium salts in order to determine the effect of sample preparation techniques on method performance using commercial herbicide formulations and (b) analysis of non-(X j,k,l (i) ) and sterilized (Y j,k,l (i) ) soil samples (i-fold rate 1, 10, 100, or 1,000; j-pesticide type A or B; k-time (0, 5, 10, 20, and 50 days) and l = 1-3 replicated samples) having clay content ∈ 5.0-12.0 %, silt ∈ 23.0-51.1 %, sand ∈ 7.2-72.0 %, and pH ∈ 4.0-8.1. In order to obtain a high representativeness of the data toward real-field experiments, the pollution scheme has involved 1-, 10-, 100-, and 1,000-fold rates. The firstfold rate has concentration of pollutant A of 2.639 × 10(-4) g in 625 cm(2) soil horizon of 0-25 cm(2) (5 cm depth) according to registration report (PSM-Zulassungbericht) of German Federal Office of Consumer Protection and Food Safety (Bundesamt für Verbraucherschutz und Lebensmittelsicherheit) 6337/26.10.2009. The experimental design has involved quincunx systematic statistical approach for collection of soil samples. The performance has been compared with the corresponding statistical variable obtained, using an independent HPLC-ESI-(APCI-)-MS/MS analysis. PMID:25555463

  16. Mass spectrometric analysis of electrophoretically separated allergens and proteases in grass pollen diffusates

    Directory of Open Access Journals (Sweden)

    Geczy Carolyn L

    2003-09-01

    Full Text Available Abstract Background Pollens are important triggers for allergic asthma and seasonal rhinitis, and proteases released by major allergenic pollens can injure airway epithelial cells in vitro. Disruption of mucosal epithelial integrity by proteases released by inhaled pollens could promote allergic sensitisation. Methods Pollen diffusates from Kentucky blue grass (Poa pratensis, rye grass (Lolium perenne and Bermuda grass (Cynodon dactylon were assessed for peptidase activity using a fluorogenic substrate, as well as by gelatin zymography. Following one- or two-dimensional gel electrophoresis, Coomassie-stained individual bands/spots were excised, subjected to tryptic digestion and analysed by mass spectrometry, either MALDI reflectron TOF or microcapillary liquid chromatography MS-MS. Database searches were used to identify allergens and other plant proteins in pollen diffusates. Results All pollen diffusates tested exhibited peptidase activity. Gelatin zymography revealed high Mr proteolytic activity at ~ 95,000 in all diffusates and additional proteolytic bands in rye and Bermuda grass diffusates, which appeared to be serine proteases on the basis of inhibition studies. A proteolytic band at Mr ~ 35,000 in Bermuda grass diffusate, which corresponded to an intense band detected by Western blotting using a monoclonal antibody to the timothy grass (Phleum pratense group 1 allergen Phl p 1, was identified by mass spectrometric analysis as the group 1 allergen Cyn d 1. Two-dimensional analysis similarly demonstrated proteolytic activity corresponding to protein spots identified as Cyn d 1. Conclusion One- and two-dimensional electrophoretic separation, combined with analysis by mass spectrometry, is useful for rapid determination of the identities of pollen proteins. A component of the proteolytic activity in Bermuda grass diffusate is likely to be related to the allergen Cyn d 1.

  17. Assessment of predictive indices for glioblastomas radiation therapy: comparison of perfusion MRI and spectrometric imagery by magnetic resonance; Evaluation d'indices predictifs pour la radiotherapie des glioblastomes: comparaison de l'IRM de perfusion et de l'imagerie de spectrometrie par resonance magnetique

    Energy Technology Data Exchange (ETDEWEB)

    Lemoine, J.M.; Laprie, A.; Moyal Cohen-Jonathan, E.; Ken, S. [Departement de radiotherapie, institut Claudius-Regaud, 31 - Toulouse (France); Lemoine, J.M.; Laprie, A.; Franceries, X.; Lotterie, J.A.; Celsis, P.; Lubrano, V.; Berry, I.; Ken, S. [Inserm, UMR 825, imagerie cerebrale et handicaps neurologiques, 31 - Toulouse (France); Lemoine, J.M.; Franceries, X. [Universite Paul-Sabatier, 31 - Toulouse (France); Lotterie, J.A.; Berry, I. [Departement de biophysique, CHU Rangueil, 31 - Toulouse (France); Lubrano, V. [Departement de neurochirurgie, CHU Rangueil, 31 - Toulouse (France)

    2010-10-15

    The authors report the comparison of several imagery modalities: anatomic imagery (T1-weighted MRI after gadolinium injection and T2-weighted MRI), metabolic imagery (spectrometric imagery by magnetic resonance) and functional imagery (perfusion MRI). This comparison has been performed within the frame of a prospective clinic test associating a radiosensitizer concomitant with a radiation therapy of glioblastomas. It appears that the integration of data of spectrometric imagery by magnetic resonance and of perfusion MRI is a promising method to overcome the resistance of glioblastomas. Short communication

  18. Calcinated gold nanoparticle arrays for on-chip, multiplexed and matrix-free mass spectrometric analysis of peptides and small molecules

    Science.gov (United States)

    Hinman, Samuel S.; Chen, Chih-Yuan; Duan, Jicheng; Cheng, Quan

    2016-01-01

    have been discussed; heat confinement and interband transition/plasmonic resonance may play important roles. Taking the accessibility of fabrication, performance, and reusability of this substrate together, the material developed here provides a new tool for multiplexed and chip-based mass spectrometric analysis. Electronic supplementary information (ESI) available: Additional methods and figures. See DOI: 10.1039/c5nr06635b

  19. iMS2Flux – a high–throughput processing tool for stable isotope labeled mass spectrometric data used for metabolic flux analysis

    Directory of Open Access Journals (Sweden)

    Poskar C Hart

    2012-11-01

    Full Text Available Abstract Background Metabolic flux analysis has become an established method in systems biology and functional genomics. The most common approach for determining intracellular metabolic fluxes is to utilize mass spectrometry in combination with stable isotope labeling experiments. However, before the mass spectrometric data can be used it has to be corrected for biases caused by naturally occurring stable isotopes, by the analytical technique(s employed, or by the biological sample itself. Finally the MS data and the labeling information it contains have to be assembled into a data format usable by flux analysis software (of which several dedicated packages exist. Currently the processing of mass spectrometric data is time-consuming and error-prone requiring peak by peak cut-and-paste analysis and manual curation. In order to facilitate high-throughput metabolic flux analysis, the automation of multiple steps in the analytical workflow is necessary. Results Here we describe iMS2Flux, software developed to automate, standardize and connect the data flow between mass spectrometric measurements and flux analysis programs. This tool streamlines the transfer of data from extraction via correction tools to 13C-Flux software by processing MS data from stable isotope labeling experiments. It allows the correction of large and heterogeneous MS datasets for the presence of naturally occurring stable isotopes, initial biomass and several mass spectrometry effects. Before and after data correction, several checks can be performed to ensure accurate data. The corrected data may be returned in a variety of formats including those used by metabolic flux analysis software such as 13CFLUX, OpenFLUX and 13CFLUX2. Conclusion iMS2Flux is a versatile, easy to use tool for the automated processing of mass spectrometric data containing isotope labeling information. It represents the core framework for a standardized workflow and data processing. Due to its flexibility

  20. Determination of Lead Content in Phosphate Rock and Concentrate Rock——Flame Atomic Absorption Spectrometric Method%火焰原子吸收光谱法测定磷矿石和精磷矿中的铅含量

    Institute of Scientific and Technical Information of China (English)

    沈治荣; 梁聪; 甘丽; 何红莲

    2011-01-01

    This article describes determination of trace harmful heavy metal-lead element in phosphate rock and concentrate rock with flame atomic absorption spectrometry method.The relative standard deviation of this method is 3.1~14.2%,recovery rate is 90%~104%,the sample detection limit is 0.0008%.The method is accurate,fast,easy,make up for method of determination lead in phosphate rock.It provides effective control method for production of feed additives and fertilizers and so on.%研究了用火焰原子吸收光谱法测定磷矿石或磷精矿中微量的铅的检测方法。此方法的相对标准偏差为3.1%-14.2%,回收率为90%-104%,样品检测下限为0.0008%。

  1. Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

    Science.gov (United States)

    Levent, Abdulkadir; Sentürk, Zühre

    2010-09-01

    Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection. PMID:20426742

  2. 静态顶空-气相色谱质谱选择性测定烟用白乳胶中7种苯系物%Selective determination of seven benzene series components in cigarette adhesives by static headspace gas chromatograph-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    姬厚伟; 刘剑; 叶冲; 万强; 韩伟; 王芳; 杨虹杰; 杨敬国

    2012-01-01

    为选择性测定烟用白乳胶中7种苯系物,建立了静态顶空-气相色谱质谱选择离子定量的测定方法.样品经140℃、30 min静态顶空后,以2-己酮为内标,采用HP-INNOWAX柱,气相色谱-质谱选择离子模式检测,内标法定量.该方法对7种苯系物的定量检测限为0.008 ~0.01 mg/kg,加标回收率为88.9%-104.5%,RSD <5%,效果良好.%A method based on static headspace gas chromatography-mass spectrometry ( SHS-GC/MS) and internal standard was developed to selectively determine seven benzene series components contents in cigarette adhesive. Experimental conditions such as headspace temperature, headspace time and analytical conditions of GC-MS were optimized. Cigarette adhesive samples were treated at 140℃ for 30 min. Head-space vapor of final extraction was injected into a HP-INNOWAX column and detected by MS. The target compounds were quantified by internal standard method under selected ion monitoring mode. Results showed that; the recoveries ranged from 88.9% to 104.5% , with relative standard deviations ( RSDs) e less than 5%. The linear range was from 0.01 to 0.5 μg/mL with a good, linear determination coefficient (R2 >0.999) and limits of quantification were 0.008 ~0.0lmg/kg. The method is accurate, simple and rapid.

  3. Mathematical treatment of mass spectrometric data for analysis of gas mixtures

    International Nuclear Information System (INIS)

    A mass spectrometric technique for gas analysis is described. To interpretate the often complex spectra, the authors propose a mathematical treatment. In a series of matrix calculations, deviations between evaluated and measured ion currents are reduced to a minimum. The necessary computer program was developed. The procedure was tested with synthetically generated mass spectra as well as with calibrated gas mixtures. It could be demonstrated that all gases in a preselected mass range, here between 1 and 60, can be determined. For individual components, the limits of detection are correlated to the degree of peak overlapping. Thus they are typical for each problem. The full range of mass spectrometric sensitivity, between 100% and about 10 ppm (vol), is accessible, when base or major peaks, which do not overlap, can be used for calculations. Otherwise, the significance of determination can be derived from the standard deviations, which are calculated with the gas fractions simultaneously

  4. Integration of landsat MSS imagery with aeromagnetic and airborne spectrometric data over a part of Mozambique

    International Nuclear Information System (INIS)

    An area within the undifferentiated Precambrian gneisses and granulites of the Mozambique Belt was studied using Landsat MSS imagery, aeromagnetic data and spectrometric data. Airborne radiometric data including total count, uranium, thorium and potassium channels and aeromagnetic data were prepared as raster scanned images, which were registered and combined with the Landsat imagery on an image processing system. In addition to study of the individual data sets the spectrometric channels were manipulated to provide ratios and composite images. These composite images provided information from the three main channels, potassium, uranium and thorium. Single channel images derived from them were colour contoured and integrated with the Landsat imagery. An interpretation of the geophysical data integrated with the Landsat imagery was compared with separate interpretations of each previously carried out. The combined display techniques employed, substantially improved the discrimination of lithology within the area studied and provided a more detailed description of the regional structure. (author). 16 refs, 6 figs, 1 tab

  5. New FORTRAN computer programs to acquire and process isotopic mass-spectrometric data

    International Nuclear Information System (INIS)

    The computer programs described in New Computer Programs to Acquire and Process Isotopic Mass Spectrometric Data have been revised. This report describes in some detail the operation of these programs, which acquire and process isotopic mass spectrometric data. Both functional and overall design aspects are addressed. The three basic program units - file manipulation, data acquisition, and data processing - are discussed in turn. Step-by-step instructions are included where appropriate, and each subsection is described in enough detail to give a clear picture of its function. Organization of file structure, which is central to the entire concept, is extensively discussed with the help of numerous tables. Appendices contain flow charts and outline file structure to help a programmer unfamiliar with the programs to alter them with a minimum of lost time

  6. Measurement techniques for trace metals in coal-plant effluents: A brief review

    Science.gov (United States)

    Singh, J. J.

    1979-01-01

    The strong features and limitations of techniques for determining trace elements in aerosols emitted from coal plants are discussed. Techniques reviewed include atomic absorption spectroscopy, charged particle scattering and activation, instrumental neutron activation analysis, gas/liquid chromatography, gas chromatographic/mass spectrometric methods, X-ray fluorescence, and charged-particle-induced X-ray emission. The latter two methods are emphasized. They provide simultaneous, sensitive multielement analyses and lend themselves readily to depth profiling. It is recommended that whenever feasible, two or more complementary techniques should be used for analyzing environmental samples.

  7. Mass Spectrometric Studies of Non-Covalent Binding Interactions Between Metallointercalators and DNA

    Science.gov (United States)

    Urathamakul, Thitima; Talib, Jihan; Beck, Jennifer L.; Ralph, Stephen F.

    Over the past 2 decades there has been increasing interest in metal complexes that bind non-covalently to DNA, driven in part by a host of potential applications for molecules that can accomplish this task with high affinity and selectivity. As a result many workers have used a wide variety of experimental techniques, several of which are discussed in other chapters of this book, to unravel the details of the precise intermolecular interactions involved. Here we discuss one of the most recent additions to the armory of techniques used by chemists to interrogate metal complex/DNA interactions. For the majority of its existence mass spectrometry (MS) has proven to be of enormous advantage to chemists by virtue of its ability to provide the molecular weights of compounds as well as structural information via fragmentation patterns. However, the high energies associated with many earlier MS techniques which result in fragmentation of covalent bonds, prevent its application for studying weaker intermolecular interactions. The advent of soft ionisation methods such as matrix assisted laser desorption ionisation (MALDI) and electrospray ionisation (ESI) has revolutionised mass spectrometric analysis of biomolecules, by allowing these normally fragile molecules to be introduced into the gas phase for analysis with minimal, if any, fragmentation. It was then recognised that ESI-MS, in particular, might be suitable for investigating non-covalent interactions between small molecules and either proteins or nucleic acids. This was confirmed by a number of early studies involving organic intercalators and minor groove binding ligands, prompting our interest in evaluating ESI-MS as a tool for studying non-covalent interactions between metal complexes and DNA. This chapter contains a discussion of the basic principles behind ESI-MS that enable it to introduce representative samples of solutions containing metal complexes and DNA into the gas phase for analysis. This will be

  8. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    International Nuclear Information System (INIS)

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 μg l-1 As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 μg l-1. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l-1 acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l-1 HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 μg l-1 for As(III) and 0.3 μg l-1 for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 μg l-1 (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non-chromatographic and chromatographic procedures and the As

  9. Aspects of optical fibers and spectrometric sensors in chemical process and industrial environments

    International Nuclear Information System (INIS)

    For on-line control, the two alternatives of automatic sample transfer and in situ remote analysis are discussed. New concepts are emerging from the possibilities offered by optical fibers. Absorption in the visible, UV and IR, fluorescence and Raman spectrometric techniques are examined. The state of the art of optodes and devices in chemical process control are given, with some examples of applications in nuclear plants

  10. Mass spectrometric analysis of the volatiles released by heating or crushing rocks

    Science.gov (United States)

    Barker, C.; Sommer, M. A.

    1973-01-01

    Vacuum extraction with subsequent mass spectrometric analysis of evolved volatiles was selected as the analytical procedure. The high-vacuum gas-handling system was constructed of stainless steel. The system was completely free from mercury, grease, or volatile organic materials. The furnace for heating the samples is discussed together with the high-vacuum crusher, the mass spectrometer, and approaches for water determination. The analytical procedure is considered, giving attention to the extraction of volatiles, adsorption studies, and the analysis of volatiles.

  11. Car-borne multichannel gamma-ray spectrometric system model CZD-6

    International Nuclear Information System (INIS)

    The car-borne multichannel gamma-ray spectrometric system Mode CZD-6 is composed of a HDY-256 of portable multichannel gamma-ray spectrometer developed by the Beijing Research Institute of Uranium Geology and a large volume scintillation detector. the position for each measurement point is determined by the GPS instrument. Its latitude and longitude, as well as measured 256 channels of γ-spectrometric data are collected by a notebook computer, which can show the 256 channels of spectra for each point during measuring processes. The complete system can be loaded in a field car. This system has been used to environmental radioactive monitoring after calibration by airborne radiometric models in Shijiazhuang, Hebei province. A lot of data confirm that the system works stably and reliably, and is a fast and advanced approach for environmental γ-spectrometric monitoring. It can be used not only to determination of contents of natural radioactive elements in environments, but also to monitoring nuclear pollution and emergency treatment in nuclear accidents significantly

  12. Novel concepts and strategies in anticancer metallodrug development : towards oral activity, peptide conjugation and mass spectrometric applications

    International Nuclear Information System (INIS)

    including top-down electrospray ionization-mass spectrometry (ESI-MS). Mass spectrometry is an invaluable tool in the analysis of molecular interactions between metallodrugs and biomolecules, such as DNA or proteins and their constituents. Furthermore, the molecular reactivity may give insight into the mode of action of a particular metallodrug or family of metallodrugs. Within the frame of this Ph.D. thesis, mass spectrometric techniques have been used to characterize the reactivity of representative (thio)pyr(id)onato RuII–p-cymene metallodrugs towards amino acids, nucleotides and proteins and an inverse correlation was found between extent of protein binding and antiproliferative activity, at least for these families of metallodrugs. Furthermore, the analysis of metallation sites of metallodrugs on proteins by mass spectrometric methods poses significant challenges in many cases due to low adduct detection efficiencies. Top-down mass spectrometric analysis is a promising approach to determine oxaliplatin binding sites on ubiquitin and different fragmentation techniques were investigated with the combination of higher energy C-trap dissociation (HCD) and electron transfer dissociation (ETD) tandem mass spectrometry yielding the highest information content. This approach led to the confirmation of methionine-1 as the primary and histidine-68 as the secondary binding site. (author)

  13. Precise determination of magnesium and lutetium in input accountability tank solutions of nuclear reprocessing plants by the mass spectrometric stable isotope dilution technique

    International Nuclear Information System (INIS)

    This paper describes the procedures for the determination of Mg and Lu concentrations in input solutions of nuclear fuel dissolved in reprocessing plants. The main aim of this work is to supply an independent method for measuring the volume of input accountability tanks. The methods used include suitable radiochemical separations and isotope dilution mass spectrometric measurements. Chemical separations from highly radioactive solutions have been tested in order to obtain pure and ''cold'' samples of Mg and Lu to be measured by Mass Spectrometry. Different ionisation techniques have been used in obtaining precise isotopic ratios. Results are presented and compared with historical data. A critical evaluation of methods, results and apparatus is given. 17 refs

  14. The IDA-80 measurement evaluation programme on mass spectrometric isotope dilution analysis of uranium and plutonium. Vol. 1

    International Nuclear Information System (INIS)

    The main objective was the acquisition of basic data on the uncertainties involved in the mass spectrometric isotope dilution analysis as applied to the determination of uranium and plutonium in active feed solutions of reprocessing plants. The element concentrations and isotopic compositions of all test materials used were determined by CBNM and NBS with high accuracy. The more than 60000 analytical data reported by the participating laboratories were evaluated by statistical methods applied mainly to the calculation of estimates of the variances for the different uncertainty components contributing to the total uncertainty of this analytical technique. Attention was given to such topics as sample ageing, influence of fission products, spike calibration, ion fractionation, Pu-241 decay correction, minor isotope measurement and errors in data transfer. Furthermore, the performance of the 'dried sample' technique and the 'in-situ' spiking method of undiluted samples of reprocessing fuel solution with U-235/Pu-242 metal alloy spikes, were tested successfully. Considerable improvement of isotope dilution analysis in this safeguards relevant application during the last decade is shown as compared to the results obtained in the IDA-72 interlaboratory experiment, organized by KfK in 1972 on the same subject. (orig./HP)

  15. 基于阳离子交换-反相混合分离模式的液相色谱-质谱联用检测河豚毒素新方法%Determination of tetrodotoxin using a cation exchange-reverse phase liquid chromatography-mass spectrometric method

    Institute of Scientific and Technical Information of China (English)

    刘希; 陈佳; 刘勤; 郭磊; 毛军文; 谢剑炜

    2012-01-01

    Objective To establish a highly sensitive method suitable for detection of intoxicated biomedical samples with regard to tetrodotoxin ,one of the most toxic non-proteins as well as a hydrophilic small biotoxin . Methods A novel method for detection of tetrodotoxin in human blood plasma by liquid chromatography -time of flight/mass spectrometry ( LC-TOF/MS) technique was established using a cation exchange -reverse phase separation mode. The LC-MS analysis and extraction conditions were systematically optimized. Results For the tetrodotoxin standard sample , the linear calibration curve ranged from 0.1 to 50 mg/L and the limit of detection ( LOD) was 0.01 mg/L. For the tetrodotoxin exposed human plasma sample, the linear calibration curve ranged from 0.5 to 10 mg/L and the LOD was 0.25 mg/L, respectively. Conclusion Such an LC-TOF/MS established for the detection of tetrodotoxin is highly specific and sensitive , and it can be feasible for the detection of tetrodotoxin at mg/L level in puffer fish biosamples.%目的 建立一种可用于检测中毒生物医学样品中小分子生物毒素--河豚毒素的高灵敏度分析方法.方法 选用阳离子交换-反相混合色谱柱,针对河豚毒素亲水性强的特点,建立了一种新型的液相色谱-飞行时间质谱方法对人血浆中河豚毒素进行检测,优化了液相色谱-质谱条件,考察了血浆中河豚毒素的提取方法.结果 对于参考品溶液,河豚毒素的线性范围为0.1~50 mg/L,检测限为0.01 mg/L;对于染毒人血浆样品,河豚毒素的线性范围为0.5~10 mg/L,检测限为0.25 mg/L.结论 所建立的液相色谱-飞行时间质谱方法专属性强、灵敏度高,可适用于实际测定河豚鱼头样品中 mg/L水平的河豚毒素.

  16. Seasonal variations of bisphenol A in the Danube River by the municipality of Novi Sad, Serbia

    Directory of Open Access Journals (Sweden)

    Milanović Maja

    2016-01-01

    Full Text Available Seasonal variations of bisphenol A (BPA were investigated in the Danube along the Novi Sad bank, Serbia using solid-phase extraction followed by gas chromatographic mass spectrometric method. The obtained results confirmed the presence of BPA above the limit of quantification (6 ng/L in 22 out of 32 water samples at all eight sampling sites. Тhe BPA concentration varied from 1 for autumn, spring and summer. The high potential risk which is attributed to the elevated summer concentrations is probably the result of the increased human activates and weather conditions. [Projekat Ministarstva nauke Republike Srbije, br. III46009

  17. Confirmation of phorate, terbufos, and their sulfoxides and sulfones in water by capillary gas chromatography/chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    A gas chromatographic/mass spectrometric method capable of confirming phorate, terbufos, their sulfoxides, and sulfones in water is reported. Parents and their metabolites are separated in less than 5 min using a short capillary GC column and high carrier gas linear velocities. Positive ion chemical ionization mass spectrometry generates (M + H) ions indicative of the different molecular weights of the analytes and at least one confirmatory fragment ion for each analyte. Residues have been qualitatively confirmed at the 1 ppb level in fortified water samples from a variety of sources. Apparent residues in control water were less than 0.1 ppb

  18. 氯霉素类三甲基硅衍生物的质谱特征及其残留监测

    Institute of Scientific and Technical Information of China (English)

    贺利民; 曾振灵; 刘雅红; 陈建新; 黄显会

    2004-01-01

    Mass characteristics of TMS derivative of chloramphenicol, florfenicol,and thiamphenicol were interpreted manually, respectively. Then SIM mode was performed at m/z 225, m/z 242, m/z 244, m/z 361 for CAP, m/z 178, m/z 257, m/z 259, m/z 394 for FF,and m/z 242, m/z 244, m/z 257, m/z 330 for TAP. A sensitive, reproducible gas chromatographic-mass spectrometric method was developed for simultaneous monitoring residues of fenicols in pork and tissues.

  19. Pharmacokinetic comparison of seven 8-methoxypsoralen brands

    DEFF Research Database (Denmark)

    Menne, T; Andersen, Klaus Ejner; Larsen, E;

    1981-01-01

    The pharmacokinetics of seven 8-MOP brands were evaluated in 7 volunteers using an incomplete bloc design. After a single oral dose the 8-MOP plasma level was followed for 3 hours. The plasma concentration was measured with a gas chromatographic - mass spectrometric method, using an isotopic...... dilution technique. The different brands could be divided into three groups. Two gave a high maximum concentration, four a medium, and one a low concentration. The large interbrand variation observed in this study can explain the variations in the results of the treatment and the differing numbers...

  20. A comparison of semiconductor gamma spectrometric analysis using the peak net area calculations and the whole spectrum processing

    International Nuclear Information System (INIS)

    This study was conducted to compare the results of gamma spectrometric analysis using the Scaling Confirmatory Factor Analysis (SCFA) method to that of Genie2K, which uses a more traditional method. Gamma ray spectra had had been acquired for several gamma standard sources, all of which except Co-57 and Eu-152 being single gamma ray emitting nuclides. These standard sources spanned the energy range from 60 keV (Am-241) to 1116 keV (Zn-65). The standard sources were counted at 3 different geometries at 3 different geometries, with source-detector distances of 0, 5, and 15 cm. Using single gamma ray spectra collected at a given counting geometry, and the certificate file, an efficiency calibration was created for that geometry. Three different test spectra, one for each counting geometry, had been created by combining several of the standard source spectra. The efficiency calibrations created for the 3 geometries were loaded into the respective spectrum files. Each test spectrum was analyzed using the standard Genie2K engines; Peak locate, Peak search, Interactive peak fit, Background subs-traction, Efficiency correction, and Nuclide Identification with interference analysis. The results of the various calculation steps were reported. In all 3 test cases, the SCFA method identified all the nuclides correctly. The K-40 activities calculated by the SCFA method were reasonably close to that from Genie2K analysis. In general, the quantitative results of the SCFA method were impressive in all 3 cases. On a positive note, the SCFA method did identify low yield gamma lines in Eu-152, which were not identified by the Genie2K analysis. This substantiates claim that the SCFA is more sensitive than the traditional method of spectrum analysis. (authors)

  1. MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission: results and performance

    Science.gov (United States)

    Buch, A.; Pinnick, V. T.; Szopa, C.; Grand, N.; Humeau, O.; van Amerom, F. H.; Danell, R.; Freissinet, C.; Brinckerhoff, W.; Gonnsen, Z.; Mahaffy, P. R.; Coll, P.; Raulin, F.; Goesmann, F.

    2015-10-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquiring samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular and chiral) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis/chemical derivatization gas chromatography (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide information on elemental and molecular makeup, polarity, chirality and isotopic patterns of analyte species. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatographymass spectrometry (GC-MS) mode of operation.

  2. Miniature Gas Chromatograph Mass Spectrometer for In-Situ Resource Utilization Project

    Data.gov (United States)

    National Aeronautics and Space Administration — In situ resource utilization (ISRU) is essential for several of NASA's future flagship missions. Currently envisioned ISRU plants include production of oxygen from...

  3. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    Science.gov (United States)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

    2014-10-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV-VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg- 1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

  4. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    International Nuclear Information System (INIS)

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg−1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm

  5. Quantitative analysis of flavonols, flavones, and flavanones in fruits, vegetables and beverages by high-performance liquid chromatography with photo-diode array and mass spectrometric detection

    DEFF Research Database (Denmark)

    Justesen, U.; Knuthsen, Pia; Leth, Torben

    1998-01-01

    A high-performance liquid chromatographic (HPLC) separation method viith photo-diode array (PDA) and mass spectrometric (MS) detection was developed to determine and quantify flavonols, flavones, and flavanones in fruits, vegetables and beverages. The compounds were analysed as aglycones, obtained...... after acid hydrolysis of freeze-dried food material. Identification was based on retention time, UV and mass spectra by comparison with commercial standards, and the UV peak areas were used for quantitation of the flavonoid contents. Examples of HPLC-MS analyses of orange pulp, tomato, and apple are...... presented. The method has been used to screen foods on the Danish market, and the contents of flavones, flavonols, and flavanones were measured. (C) 1998 Elsevier Science B.V....

  6. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements

    DEFF Research Database (Denmark)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin;

    2014-01-01

    This paper reports an analytical method for the determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation...... counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5×105 for 20 g soil compared to the level reported in the literature......, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference...

  7. Atomic-absorption spectrometric determination of cobalt, nickel, and copper in geological materials with matrix masking and chelation-extraction

    Science.gov (United States)

    Sanzolone, R.F.; Chao, T.T.; Crenshaw, G.L.

    1979-01-01

    An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO3 and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5-1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature. ?? 1979.

  8. Characterization of used lubricating oil by spectrometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Andressa Moreira de, E-mail: andressa@ctaa.embrapa.br [Embrapa Agroindustria de Alimentos, Guaratiba, Rio de Janeiro, RJ (Brazil); Correa, Sergio Machado [Faculdade de Engenharia. Universidade do Estado do Rio de Janeiro (UERJ), Resende, RJ (Brazil); Silva, Glauco Correa da [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2011-07-01

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer{sup R} OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu{sup R} model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100{mu}A, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics

  9. Characterization of used lubricating oil by spectrometric techniques

    International Nuclear Information System (INIS)

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-ElmerR OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX ShimadzuR model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

  10. Computational modelling of field distribution of spectrometric magnet

    International Nuclear Information System (INIS)

    Design, construction and operation of magnetic systems of some electrophysical setups require a preliminary mathematical modelling. While calculating the fields of the mentioned magnetic systems (on the base of solving a set of the direct problems of magnetostatics), we are concerned with solving the inverse problem of magnetostatics, namely, with finding an optimal construction of the current elements and ferromagnetic yoke for the required distribution of the magnetic field. In the present work a method of refinement of numerical solution to magnetostatic problem for the area with the boundaries containing the 'corner points' is proposed. The method stated above was used for the numerical simulation of a set of modifications of the magnetic system SP-94 used in some experimental setups

  11. Rapid identification of viridans streptococci by mass spectrometric discrimination.

    OpenAIRE

    Friedrichs, C.; Rodloff, A C; Chhatwal, G. S.; Schellenberger, W; Eschrich, K

    2007-01-01

    Viridans streptococci (VS) are responsible for several systemic diseases, such as endocarditis, abscesses, and septicemia. Unfortunately, species identification by conventional methods seems to be more difficult than species identification of other groups of bacteria. The aim of the present study was to evaluate the use of cell matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF-MS) for the rapid identification of 10 different species of VS. A total of 99 V...

  12. Heater-induced ionization inferred from spectrometric airglow measurements

    Science.gov (United States)

    Hysell, D. L.; Miceli, R. J.; Varney, R. H.; Schlatter, N.; Huba, J. D.

    2013-12-01

    Spectrographic airglow measurements were made during an ionospheric modification experiment at HAARP on March 12, 2013. Artificial airglow enhancements at 427.8, 557.7, 630.0, 777.4, and 844.6 nm were observed. On the basis of these emissions and using a methodology based on the method of Backus and Gilbert [1968, 1970], we estimate the suprathermal electron population and the subsequent equilibrium electron density profile, including contributions from electron impact ionization. We find that the airglow is consistent with significant induced ionization in view of the spatial intermittency of the airglow.

  13. Inclusion of riboflavin in β-cyclodextrin: A fluorimetric and absorption spectrometric study

    Science.gov (United States)

    Roy, Dalim Kumar; Deb, Nipamanjari; Ghosh, Bankim Chandra; Mukherjee, Asok K.

    2009-07-01

    Formation of inclusion complexes between riboflavin and β-cyclodextrin (β-CD) with both 1:1 and 1:2 stoichiometry has been established by fluorimetric titration. However, in absorption spectrometric experiment, spectral change of riboflavin in the visible range could be observed only by taking β-CD at a much higher concentration (about 100 times) than riboflavin and under such condition only 1:2 complexes could be detected. Its formation constant ( K) was determined by a multiple linear regression analysis of the absorption data. The reliability of the K value was confirmed by the consistency achieved on analyzing the data at two different wavelengths.

  14. Mass spectrometric studies on irradiated (U, Pu) mixed carbide fuel of Fbtr

    Energy Technology Data Exchange (ETDEWEB)

    Balasubramanian, R. [Fuel Chemistry Division, IGCAR, Kalpakkam 603 102, Tamil Nadu (India)]. E-mail: rbs@igcar.ernet.in; Darwin Albert Raj, D.; Nalini, S.; Sai Baba, M. [Fuel Chemistry Division, IGCAR, Kalpakkam 603 102, Tamil Nadu (India)

    2005-07-01

    Mass spectrometry was employed to characterise the irradiated mixed carbide fuel of fast breeder test reactor (FBTR) for assessing its performance: thermal ionisation mass spectrometry to determine the isotopic composition, concentrations of U, Pu and Nd in the dissolver solutions and to deduce the burn-up, and a quadrupole mass spectrometric system to obtain the percentage release of fission gases (Kr + Xe). A summary and analysis of the results obtained with the fuel at 25,000 and 50,000 MWd/t in these studies is given in this paper. (author)

  15. Spectrometric scintillation units for gamma detection based on oxide scintillators with great atomic number

    International Nuclear Information System (INIS)

    Gamma-radiation detecting scintillation spectrometric units based on monocrystals of bismuth germanate (BGO) and cadmium tungstate (CWO) were developed to carry out express control of the environment migration of radionuclides. Detecting unit includes a BGO or CWO detector, FEU-176, supply voltage high-volt converter, amplifier-oscillator and differential discriminator to separate radionuclides. BGO base scintillation detecting unit with 40 x 40 mm dimensions has following parameters as to 137 Cs: amplitude resolution - 12.4%; recording efficiency - 45%; sensitivity - 0.004 pulse/Bq x s. The level of specific background with passive protection - 0.55 pulse/s

  16. Mass spectrometric studies on irradiated (U, Pu) mixed carbide fuel of Fbtr

    International Nuclear Information System (INIS)

    Mass spectrometry was employed to characterise the irradiated mixed carbide fuel of fast breeder test reactor (FBTR) for assessing its performance: thermal ionisation mass spectrometry to determine the isotopic composition, concentrations of U, Pu and Nd in the dissolver solutions and to deduce the burn-up, and a quadrupole mass spectrometric system to obtain the percentage release of fission gases (Kr + Xe). A summary and analysis of the results obtained with the fuel at 25,000 and 50,000 MWd/t in these studies is given in this paper. (author)

  17. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.; With, T. K.

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal compl...... complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro...

  18. Carborne gamma-ray spectrometric survey of an area east of Homs, central Syria

    International Nuclear Information System (INIS)

    A carborne gamma-ray spectrometric survey normally provides preliminary reconnaissance coverage of the radioelements in the topmost part of the earth's crust. However, a radiometric survey under certain conditions can be used for geologic mapping. In the present paper this approach was used to differentiate various lithological units within the Neogene formations east of Homs. The total radioactivity and the ground concentrations of potassium, uranium, and thorium were obtained over an area of 294 km2. Despite, generally, the small variations in the contents of these variables, it was possible to categorize some rock units in the study area based on their radiometric response. (Author)

  19. Double-comparison method for mass spectrometric determination of hydrogen isotopic abundances

    International Nuclear Information System (INIS)

    Hydrogen isotope ratio analysis is subject to interference from H3+, and the uncertainty in the H3+ correction is generally the limiting factor in the precision of hydrogen isotopic analyses. Mathematical modeling indicates that the precision of the analysis can be improved through the use of a double-comparison technique employing a second reference gas. In order to compare the single- and double-comparison techniques, a double-collector isotope ratio mass spectrometer was fitted with a triple viscous leak inlet system. Four H2 samples with deuterium contents between -184 and 193% vs. standard mean ocean water were analyzed by both techniques. The single-comparison analysis had a precision of about 1%. The double-comparison analysis had a precision of 0.04% when combined with electrical H3+ correction. When no H3+ correction was used in the double-comparison measurements, the precision varied as a function of degree of mismatching of major ion currents of the unknown and reference gases and was frequently as poor as .05%

  20. Determination of the X-Ray generators ripples 'at constant voltage' by the spectrometric method

    International Nuclear Information System (INIS)

    The ripple measurement of three X-Ray generator, using a traditional sectrometric system, in coincidence with the control pulse is done. The sweeping is done at the T oscillation period in the feeding network of the X-Ray generator. The generators used were from Siemens, two with medium energy and one with low energy, all with complete wave retification. (E.G.)

  1. Heterogeneous nuclear ribonucleoproteins C1/C2 identified as autoantigens by biochemical and mass spectrometric methods

    DEFF Research Database (Denmark)

    Heegaard, N H; Larsen, Martin Røssel; Muncrief, T;

    2000-01-01

    gel and their contents were analyzed by matrix-assisted laser desorption-ionization (MALDI) or nanoelectrospray ionization time-of-flight (TOF) tandem mass spectrometry (MS) after in-gel digestion with trypsin. A database search identified the proteins as the C1 and C2 heterogeneous nuclear...

  2. A computer program for nuclear fuel burnup determination using gamma spectrometric methods

    International Nuclear Information System (INIS)

    In the end of its service life in the reactor, the fuel needs to be characterized for reasons relating both to safety and economy. The main investigations carried out are oriented towards verifying the fuel cladding integrity and determining the fissile content and the fuel burnup. A computer program for fast burnup evaluation was developed at the Post-Irradiation Examination Laboratory (PIEL) from INR Pitesti, the only laboratory of this kind in Romania. The input data consists, on one hand, of axial and radial gamma-scanning profiles (for the experimental evaluation of the number of nuclei of a given fission product - selected as burnup monitor - in the end of irradiation) and, on the other hand, of the history of irradiation (the time length and relative value of the neutron flux for each step of irradiation). Using the equation for the build-up and decay of the burnup monitor during irradiation the flux value is iteratively adjusted until the calculated number of nucleus is equal to the experimental one. Then the flux value is used in the equations of evolution of the fissile and fertile nuclei to determine the number of fissions and consequently the fuel burnup. The program was successfully used in the analysis of more then one hundred of TRIGA and CANDU-type fuel rods. An experimental result is reported in some details. (authors)

  3. [Mass Spectrometric Methods for Colorative Mechanism Analysis of Yaozhou Porcelain Glaze].

    Science.gov (United States)

    Xiao, Yuan-fang; He, Miao-hong; Zhang, Shu-di; Hang, Wei

    2015-09-01

    An in-house-built femtosecond laser ionization time-of-flight mass spectrometry (fs-LI-TOFMS) has been applied to the multi-elemental analysis of porcelain glaze from Yaozhou kiln. The samples are selected representing products of different dynasties, including Tang, Five, Song, Jin, and Ming Dynasty. For exploring the colorative mechanism of Yaozhou porcelain through the elemental analysis of the glaze, the effects of all potential coloring elements, especially transition elements, were considered. There was a speculation that the typical Co-Cr-Fe-Mn recipe was used in the fabrication of Yaozhou black glaze; the low content of Fe and high content of Ni resulted in the porcelain of white glaze; an increase content of P could lead the porcelain to be yellow-glazed. Undoubtedly, this research is an important supplement to the study of the colorative mechanism of the Yaozhou porcelain system. PMID:26669145

  4. Urban air pollution and its photochemistry studied by laser spectrometric methods

    Czech Academy of Sciences Publication Activity Database

    Zelinger, Zdeněk; Kubát, Pavel; Střižík, M.; Bezpalcová, Klára; Jaňour, Zbyněk; Danihelka, P.; Drábková, S.; Kozubková, M.; Berger, P.; Černý, A.; Engst, P.

    Dordrecht: Springer, 2006 - (Perrin, A.; Sari Zizi, N.; Demaison, J.), s. 301-316. (NATO Security through Science Series C. Environmental Security). ISBN 1-4020-5088-7. [NATO Advanced Research Workshop on Remote Sensing of the Atmosphere for Environmental Security. Rabat (MA), 16.11.2005-19.11.2005] R&D Projects: GA MŠk OC 723.001; GA MŠk 1P05ME766 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z20760514 Keywords : air pollution * differential absorption LIDAR * physical modelling Subject RIV: CF - Physical ; Theoretical Chemistry

  5. Neutron spectrometric evaluations in the Argentine research reactor RA-1

    International Nuclear Information System (INIS)

    Full text: The determination of the quantities dose equivalent H*(10) and personal dose equivalent Hp(10) in mixed field (n,γ) needs the knowledge of the related spectrum. In order to fulfill this aim spectrometer system has been built based on the combination of polyethylene spheres of different diameters (Bonner Spheres System-BSS) and a He3 proportional counter detector sensitive to thermal neutrons. The detector is located in the geometrical centre of each of the spheres and has an associated electronics with a charge preamplifier, an amplifier and a multichannel system that allows the outgoing spectrum analysis. In order to determine the neutron spectrum a deconvolution method is applied based on the LOUHI82 code. In this work are shown the spectra and the related values of H*(10) that have been got in five places of the reactor and in the command room with the BSS. (author)

  6. Mass spectrometric analysis with cluster projectiles and coincidence counting

    Energy Technology Data Exchange (ETDEWEB)

    Cox, B.D.

    1992-01-01

    Methods for maximizing the amount of secondary ion information, per primary projectile, are described. The method is based on time-of-flight mass spectrometry and event-by-event coincidence counting. The information obtained from coincidence counting time-of-flight mass spectrometry includes: (a) surface composition, (b) relative concentrations, and (c) degree of intermolecular mixing. The technique was applied to the study of an important new class of polymers: polymer blends. Secondary ion mass spectrometry, when applied to the analysis of synthetic polymers, induces backbone fragmentation which is characteristic of the homopolymer. The characteristic fingerprint peaks from polystyrene and poly(vinyl methyl ether) were used to identify the presence of these two polymers in a polymer blend. The percent coincidence between the characteristic secondary ions from each component of the blend were used to determine both the relative concentration and the degree of molecular mixing. Results indicate molecular segregation of the two polymers on the film surface. The largest degree of segregation was determined for the phase separated blends. The performance of this technique depends on the desorption efficiency of the primary projectiles. In practice one seeks primary ions which are surface sensitive, have controllable parameters such as size, velocity, and charge state, and generate high secondary ion yields. Focus was placed on the use of keV organic cluster projectiles to meet these criteria. Of interest to this study were C[sub 18] (chrysene), C[sub 24] (coronene), and C[sub 60] (buckminster-fulleren). Results indicate enhanced secondary ion yields for C[sub 60]. For example, when CsI is bombarded with 30 keV C[sub 60], the yields for I[sup [minus

  7. The fuel burn-up determination by combined passive neutron and gamma - spectrometric ND - measurements. Final report for the period 1 July 1980 - 30 April 1988

    International Nuclear Information System (INIS)

    The non-destructive gamma-spectrometric method (HRGS) and the passive neutron technique (PNT) were applied to the determination of WWER 440 reactor spent fuel assemblies burn-up for safeguard purposes. Rapid codes FISPR-2 and BUNECO were compiled on HP-85 and OLIVETTI M24 computers for the IAEA inspectors. An improved equipment was constructed and tested for the fixation of the ''fork detector''. Measurements were carried-out at 1st unit of NPP Bohunice. The correlation between burn-up and fission product ratio 134Cs/137Cs or neutron count rate were analysed. Correlations between concentrations 235U, Pu and burn-up were analysed as well. A simplified procedure for assemblies burn-up check by PNT was proposed for the inspectors. Refs, figs and tabs

  8. The synthesis, mass spectrometric properties and identification of some N,N-di-(β-arylisopropyl)formamides related to the synthesis of ring-modified amphetamines.

    Science.gov (United States)

    Błachut, Dariusz; Danikiewicz, Witold; Wojtasiewicz, Krystyna; Olejnik, Marian; Kalinowska, Iwona; Szawkało, Joanna; Czarnocki, Zbigniew

    2011-03-20

    This study examines the electron impact (EI) induced mass spectrometric behavior of several N,N-di-(β-arylisopropyl)formamides, which are connected to the Leuckart synthesis of some amphetamine analogues. Emphasis is laid on the fragmentation paths, which are common for all compounds under investigation and may be used in construction of the prediction scheme useful for identification of similar impurities, especially in absence of desirable authentic material. On the basis of this scheme several new N,N-di-(β-arylisopropyl)formamides have been identified in selected amphetamine analogues synthesized by the Leuckart method, including 4-methylthioamphetamine (4-MTA), 4-fluoroamphetamine (4-FA), 4-methylamphetamine, 3-trifluoromethylamphetamine, 3,4-methylenedioxyamphetamine (MDA), 2,5-dimethoxyamphetamine (2,5-DMA), 2,4,5- and 3,4,5-trimethoxyamphetamines (2-TMA and 3-TMA). PMID:20846801

  9. Thermospray ionization mass spectrometric characterization on thermal stability of developing pharmaceutical products; TSP shitsuryo bunsekiho ni yoru kaihatsu iyakuhin no netsuanteisei hyoka no kokoromi

    Energy Technology Data Exchange (ETDEWEB)

    Nishimura, T.; Ishizuka, Y. [Pharmacia and Upjohn Tsukuba Research Lab., Tsukuba (Japan)

    1998-08-01

    In order to ensure quality of pharmaceutical products, the data concerning stability of pharmaceutical products are a kind of important parameters. It is well known that hydrolytic ion peaks caused by heat at initial stage appear in the positions that do not correspond to the molecular ion peaks according to the thermospray ionization LC/MS. It is an obstacle for obtaining high quality LC/MS data, and it is necessary to minimize it by restraining the spray temperature. In this study, using thermospray ionization mass spectrometric analyzer, re-evaluation of an on-line investigation method of pharmaceutical products in solution is studied. And, an example of its application, namely, an application on two kinds of pharmaceutical products, PNU-52047 that is a kind of anticancer drugs (USAN name: Menogaril) and PNU-100766 that is antibiotic material used for mesitylene resistance yellow staphylococcus (MRSA) that is a reason of in hospital inflection, is illustrated. 6 refs., 7 figs.

  10. Mass spectrometric measurements of the isotopic anatomies of molecules (Invited)

    Science.gov (United States)

    Eiler, J. M.; Krumwiede, D.; Schlueter, H.

    2013-12-01

    Site-specific and multiple isotopic substitutions in molecular structures potentially provide an extraordinarily rich set of constraints on their sources, conditions of formation, reaction and transport histories, and perhaps other issues. Examples include carbonate ';clumped isotope' thermometry, clumped isotope measurements of CO2, O2, and, recently, methane, ethane and N2O; site-specific 15N measurements in N2O and 13C and D analyses of fatty acids, sugars, cellulose, food products, and, recently, n-alkanes. Extension of the principles behind these tools to the very large number of isotopologues of complex molecules could potentially lead to new uses of isotope chemistry, similar to proteomics, metabolomics and genomics in their complexity and depth of detail (';isotomics'?). Several technologies are potentially useful for this field, including ';SNIF-NMR', gas source mass spectrometry and IR absorption spectroscopy. However, all well established methods have restrictive limits in the sizes of samples, types of analyzes, and the sorts of isotopologues that can be measured with useful precision. We will present an overview of several emerging instruments and techniques of high-resolution gas source mass spectrometry that may enable study of a large proportion of the isotopologues of a wide range of volatile and semi-volatile compounds, including many organics, with precisions and sample sizes suitable for a range of applications. A variety of isotopologues can be measured by combining information from the Thermo 253 Ultra (a new high resolution, multi-collector gas source mass spectrometer) and the Thermo DFS (a very high resolution single collector, but used here on a novel mode to achieve ~per mil precision ratio measurements), sometimes supplemented by conventional bulk isotopic measurements. It is possible to design methods in which no one of these sources of data meaningfully constrain abundances of specific isotopologues, but their combination fully and

  11. Mass spectrometric studies on Ce-Cd system

    International Nuclear Information System (INIS)

    Molten salt electrorefining process, which is a pyrochemical reprocessing method, is ideally suited for reprocessing of metallic fuels. Separation of fuel material and fission products is carried out by electrorefining of spent fuel by using solid mandrel and liquid cadmium as cathodes for the electrodeposition of uranium and transuranium elements, respectively. Due to the standard electrode potentials of rare earths being close to that of transuranium elements, some amount of rare-earths are accompanied during the electrodeposition of Pu and minor actinides at liquid cadmium cathode. Therefore the investigation of thermodynamic properties of rare earth-cadmium system is essential. As part of this, vaporization studies on Ce-Cd system with the initial composition of 63.3 at % Cd (corresponding to Cd2Ce+CdCe phase region) has been investigated by Knudsen effusion mass spectrometry. This paper reports the preliminary studies carried out on this system. High purity cadmium (99.99%, M/s. Johnson Matthey Chemical Ltd, England) and cerium (99.8%, M/s. Alfa Aesar) were used for the preparation. The sample was prepared by isopiestic method by equilibrating Cd vapours over the Ce samples in a vacuum sealed quartz set up kept in a gradient furnace. The quartz set up was subsequently quenched and opened inside an argon atmosphere glove box to retrieve the sample. The phase characterization was carried out by XRD. A VG Micromass 30 BK mass spectrometer was employed for the vaporisation studies. The sample was taken in an alumina Knudsen cell (Sample loading carried out inside an argon atmosphere glovebox) and this was placed inside a molybdenum outer cup and a tungsten lid. The cell was heated by electron bombardment and the vapour effusing from Knudsen cell was ionized by electron impact, the ions produced were mass analysed by a 90° sector magnetic analyser and detected by a secondary electron multiplier. Cd+ was the ion detected in the mass spectra of the equilibrium

  12. Spectrometric assessment of thyroid depth within the radioiodine test; Spektrometrisches Verfahren zur Tiefenbestimmung der Schilddruese im Rahmen des Radioiodtests

    Energy Technology Data Exchange (ETDEWEB)

    Rink, T.; Bormuth, F.-J.; Schroth, H.-J.; Braun, S.; Zimny, M. [Klinikum Stadt Hanau (Germany). Abt. fuer Nuklearmedizin

    2005-07-01

    Aim of this study is the validation of a simple method for evaluating the depth of the target volume within the radioiodine test by analyzing the emitted iodine-131 energy spectrum. Patients, methods: In a total of 250 patients (102 with a solitary autonomous nodule, 66 with multifocal autonomy, 29 with disseminated autonomy, 46 with Graves' disease, 6 for reducing goiter volume and 1 with only partly resectable papillary tyhroid carcinoma), simultaneous uptake measurements in the Compton scatter (210{+-}110 keV) and photopeak (364-45/+55 keV) windows were performed over one minute 24 hours after application of the 3 MBq test dose, with subsequent calculation of the respective count ratios. Measurements with a water-filled plastic neck phantom were carried out to perceive the relationship between these quotients and the average source depth and to get a calibration curve for calculating the depth of the target volume in the 250 patients for comparison with the sonographic reference data. Another calibration curve was obtained by evaluating the results of 125 randomly selected patient measurements to calculate the source depth in the other half of the group. Results: The phantom measurements revealed a highly significant correlation (r=0,99) between the count ratios and the source depth. Using these calibration data, a good relationship (r=0,81, average deviation 6 mm corresponding to 22%) between the spectrometric and the sonographic depths was obtained. When using the calibration curve resulting from the 125 patient measurements, the average deviation in the other half of the group was only 3 mm (12%). There was no difference between the disease groups. Conclusion: The described method allows an easy to use depth correction of the uptake measurements providing good results. (orig.)

  13. Improved spectrometric characteristics of thallium bromide nuclear radiation detectors

    CERN Document Server

    Hitomi, K; Shoji, T; Suehiro, T; Hiratate, Y

    1999-01-01

    Thallium bromide (TlBr) is a compound semiconductor with a high atomic number and wide band gap. In this study, nuclear radiation detectors have been fabricated from the TlBr crystals. The TlBr crystals were grown by the horizontal travelling molten zone (TMZ) method using the materials purified by many pass zone refining. The crystals were characterized by measuring the resistivity, the mobility-lifetime (mu tau) product and the energy required to create an electron-hole pair (the epsilon value). Improved energy resolution has been obtained by the TlBr radiation detectors. At room temperature the full-width at half-maximum (FWHM) for the 59.5, 122 and 662 keV gamma-ray photo peak obtained from the detectors were 3.3, 8.8 and 29.5 keV, respectively. By comparing the saturated peak position of the TlBr detector with that of the CdTe detector, the epsilon value has been estimated to be about 5.85 eV for the TlBr crystal.

  14. Vacuum ultraviolet photoionization mass spectrometric study of cyclohexene.

    Science.gov (United States)

    Chen, Jun; Cao, Maoqi; Wei, Bin; Ding, Mengmeng; Shan, Xiaobin; Liu, Fuyi; Sheng, Liusi

    2016-02-01

    In this work, photoionization and dissociation of cyclohexene have been studied by means of coupling a reflectron time-of-flight mass spectrometer with the tunable vacuum ultraviolet (VUV) synchrotron radiation. The adiabatic ionization energy of cyclohexene as well as the appearance energies of its fragment ions C6 H9 (+) , C6 H7 (+) , C5 H7 (+) , C5 H5 (+) , C4 H6 (+) , C4 H5 (+) , C3 H5 (+) and C3 H3 (+) were derived from the onset of the photoionization efficiency (PIE) curves. The optimized structures for the transition states and intermediates on the ground state potential energy surfaces related to photodissociation of cyclohexene were characterized at the ωB97X-D/6-31+g(d,p) level. The coupled cluster method, CCSD(T)/cc-pVTZ, was employed to calculate the corresponding energies with the zero-point energy corrections by the ωB97X-D/6-31+g(d,p) approach. Combining experimental and theoretical results, possible formation pathways of the fragment ions were proposed and discussed in detail. The retro-Cope rearrangement was found to play a crucial role in the formation of C4 H6 (+) , C4 H5 (+) and C3 H5 (+) . Intramolecular hydrogen migrations were observed as dominant processes in most of the fragmentation pathways of cyclohexene. The present research provides a clear picture of the photoionization and dissociation processes of cyclohexene in the 8- to 15.5-eV photon energy region. Copyright © 2016 John Wiley & Sons, Ltd. PMID:26889934

  15. Methods for the accountability of uranium dioxide

    International Nuclear Information System (INIS)

    Procedures for the determination of the total U and the amount of 235U isotope in UO2 powder and pellets are given. Methods for U determination include coulometry, titration, and gravimetry. Surface-ionization mass spectroscopy is described for 235U measurement. Spectrometric procedures are described for determining the impurity content in the UO2. (U.S.)

  16. The benefits and industrial experience from spectrometric borehole logging technology in the Pilbara iron ore deposits

    International Nuclear Information System (INIS)

    The CSIRO in Australia has carried out research and developed a family of borehole logging technologies known as SIROLOG which has applications to quantitative estimation in all phases of the iron ore mining industry, namely exploration, mine development and grade control in extraction. The techniques are spectrometric in relation to the detection and recording of the gamma rays which are either excited or scattered in within the ore matrix as a consequence of nuclear reactions. The spectrometric techniques developed by the CSIRO group included a gamma-gamma technique for the simultaneous determination of iron ore grade, bulk density and blast hole diameter and a neutron-gamma technique for the simultaneous determination of iron ore grade and silica contamination. In addition, the group developed both natural gamma and neutron activation techniques for determining alumina contamination. The paper discusses the instrumentation and equipment designed for manufacture by CSIRO, the methodology for calibration of probe responses against geological parameters and it presents a discussion of the results, particularly their precision and accuracy, which were obtained from routine logging operations in applications to production, exploration and mine development. (author). 10 refs., 9 figs., 2 tabs

  17. Determination of suvorexant in human plasma using 96-well liquid-liquid extraction and HPLC with tandem mass spectrometric detection.

    Science.gov (United States)

    Breidinger, S A; Simpson, R C; Mangin, E; Woolf, E J

    2015-10-01

    A method, using liquid chromatography with tandem mass spectrometric detection (LC-MS/MS), was developed for the determination of suvorexant (MK-4305, Belsomra(®)), a selective dual orexin receptor antagonist for the treatment insomnia, in human plasma over the concentration range of 1-1000ng/mL. Stable isotope labeled (13)C(2)H3-suvorexant was used as an internal standard. The sample preparation procedure utilized liquid-liquid extraction, in the 96-well format, of a 100μL plasma sample with methyl t-butyl ether. The compounds were chromatographed under isocratic conditions on a Waters dC18 (50×2.1mm, 3μm) column with a mobile phase consisting of 30/70 (v/v %) 10mM ammonium formate, pH3/acetonitrile at a flow rate of 0.3mL/min. Multiple reaction monitoring of the precursor-to-product ion pairs for suvorexant (m/z 451→186) and (13)C(2)H3-suvorexant (m/z 455→190) on an Applied Biosystems API 4000 tandem mass spectrometer was used for quantitation. Intraday assay precision, assessed in six different lots of control plasma, was within 10% CV at all concentrations, while assay accuracy ranged from 95.6 to 105.0% of nominal. Quality control (QC) samples in plasma were stored at -20°C. Initial within day analysis of QCs after one freeze-thaw cycle showed accuracy within 9.5% of nominal with precision (CV) of 6.7% or less. The plasma QC samples were demonstrated to be stable for up to 25 months at -20°C. The method described has been used to support clinical studies during Phase I through III of clinical development. PMID:26343269

  18. 质谱技术在DNA甲基化研究中的应用%Application of Mass Spectrometric Technology in DNA Methylation Study

    Institute of Scientific and Technical Information of China (English)

    黄新凤; 叶金波; 刘建军

    2015-01-01

    DNA methylation is one of most important epigenetic modifications, which mainly occurs in carbon-5 position of CpG nucleotide sequence in mammal genomes and relates to organism development, transposable silence, X chromosome inactivation and many diseases. The understanding for molecular mechanism of DNA methylation formation, maintenance and reconstruction remain limited. however, in order to find an optimal method for DNA methylation qualitative and quantitative analysis, mass spectrometric technology with high sensitivity, good performance, high precision, high resolution and good repeatability, has a great value in the study of DNA methylation. In the following, we will make a introduction of mass spectrometric technology application in whole genomic DNA methylation and promoter DNA methylation study.%DNA甲基化是最重要的表观遗传修饰之一,主要发生在哺乳动物基因组CpG核苷酸序列中的胞嘧啶C-5位点,并与机体生长发育、转座子沉默、X染色体失活及许多疾病的发生相关。但对DNA甲基化的形成、维持和重构的分子机制的认识是有限的,需要从基因组水平寻找最优的DNA甲基化定性和定量分析方法,而质谱技术以高敏感性、高通量、高准确率、高分辨率、快速且重复性好等优势在该研究领域具有较大的应用价值。介绍质谱技术在全基因组DNA甲基化和启动子区甲基化分析中的应用。

  19. An Attempt to automate the lithological classification of rocks using geological, gamma-spectrometric and satellite image datasets

    International Nuclear Information System (INIS)

    The present study aims essentially at proving that the application of the integrated airborne gamma spectrometric and satellite image data is capable of refining the mapped surface geology, and identification of anomalous zones of radioelement content that could provide favorable exploration targets for radioactive mineralizations.The application of the appropriate statistical technique to correlate between satellite image data and gamma-spectrometric data is of great significance in this respect. Experience shows that Landsat T M data in 7 spectral bands are successfully used in such studies rather than MSS. Multivariate statistical analysis techniques are applied to airborne spectrometric and different spectral Landsat T M data. Reduction of the data from n-dimensionality, both qualitatively as color composite image, and quantitatively, as principal component analysis, is performed using some statistical control parameters. This technique shows distinct efficiency in defining areas where different lit ho facies occur. An area located at the north of the Eastern Desert of Egypt, north of Hurgada town, was chosen to test the proposed technique of integrated interpretation of data of different physical nature. The reduced data are represented and interpreted both qualitatively and quantitatively. The advantages and limitations of applying such technique to the different airborne spectrometric, and Landsat T M data are identified. (authors)

  20. Spectrometric characteristics of the γ emission of fission products: analysis of irradiated uranium with a 'germanium-lithium' detector

    International Nuclear Information System (INIS)

    In order to study the γ-ray spectra of atmospheric aerosol samples obtained with Ge-Li detectors, the spectrometric characteristics of fission product γ-ray emission had first to be specified by analyzing the evolution through time of the spectra of irradiated uranium. (authors)

  1. Algorithm for comprehensive analysis of datasets from hyphenated high resolution mass spectrometric techniques using single ion profiles and cluster analysis.

    Science.gov (United States)

    Erny, Guillaume L; Acunha, Tanize; Simó, Carolina; Cifuentes, Alejandro; Alves, Arminda

    2016-01-15

    Various algorithms have been developed to improve the quantity and quality of information that can be extracted from complex datasets obtained using hyphenated mass spectrometric techniques. While different approaches are possible, the key step often consists in arranging the data into a large series of profiles known as extracted ion profiles. Those profiles, similar to mono-dimensional separation profiles, are then processed to detect potential chromatographic peaks. This allows extracting from the dataset a large number of peaks that are characteristics of the compounds that have been separated. However, with mass spectrometry (MS) detection, the response is usually a complex signal whose pattern depends on the analyte, the MS instrument and the ionization method. When converted to ionic profiles, a single separated analyte will have multiple images at different m/z range. In this manuscript we present a hierarchical agglomerative clustering algorithm to group profiles with very similar feature. Each group aims to contain all profiles that are due to the transport and monitoring of a single analyte. Clustering results are then used to generate a 2 dimensional representation, called clusters plot, which allows an in-depth analysis of the MS dataset including the visualization of poorly separated compounds even when their intensity differs by more than two orders of magnitude. The usefulness of this new approach has been validated with data from capillary electrophoresis time of flight mass spectrometry hyphenated via an electrospray ionization. Using a mixture of 17 low molecular endogenous compounds it was verified that ionic profiles belonging to each compounds were correctly clustered even with very low degree of separation (R below 0.03). The approach was also validated using a urine sample. While with the total ion profile 15 peaks could be distinguished, 70 clusters were obtained allowing a much thorough analysis. In this particular example, the total

  2. Terverticillate Penicillia studied by direct electrospray mass spectrometric profiling of crude extracts: I. Chemosystematics

    DEFF Research Database (Denmark)

    Smedsgaard, Jørn; Frisvad, Jens Christian

    1997-01-01

    mass profile, but a noise level was applied. Cluster analysis using the correlation coefficient resulted in dendrograms where approximately 75% of the included taxa could be considered segregated in distinct clusters. Standard normalized data (mass spectra) resulted in clear clusters, but grouped taxa......A chemosystematic study of 339 isolates from all known terverticillate Penicillium taxa was performed using electrospray mass spectrometric analysis of extractable metabolites. The mass profiles were made by injecting crude plug extracts made from cultures grown on Czapek Yeast Autolysate agar (CYA......) and Yeast Extract Sucrose agar (YES) directly into the electrospray source of the mass spectrometer. A data matrix was made from each substrate by transferring the complete centroid mass spectrum from 200 to 700 amu as 501 variables to individual columns. No attempt was made to identify ions in the...

  3. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.;

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal...... complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro......-prophyrin permethylester were all found to have the same molecular ion sensitivities as their metal-free porphyrin ester. The relative metalloporphyrin ester content in a sample of porphyrin ester was thus obtained directly as the integrated ion current ratios of the normalized molecular ions. The preparation of...

  4. Laser Spectrometric Measurement System for Local Express Diagnostics of Flame at Combustion of Liquid Hydrocarbon Fuels

    Science.gov (United States)

    Kobtsev, V. D.; Kozlov, D. N.; Kostritsa, S. A.; Smirnov, V. V.; Stel'makh, O. M.; Tumanov, A. A.

    2016-03-01

    A laboratory laser spectrometric measurement system for investigation of spatial distributions of local temperatures in a flame at combustion of vapors of various liquid hydrocarbon fuels in oxygen or air at atmospheric pressure is presented. The system incorporates a coherent anti-Stokes Raman spectrometer with high spatial resolution for local thermometry of nitrogen-containing gas mixtures in a single laser shot and a continuous operation burner with a laminar diffusion flame. The system test results are presented for measurements of spatial distributions of local temperatures in various flame zones at combustion of vapor—gas n-decane/nitrogen mixtures in air. Its applicability for accomplishing practical tasks in comparative laboratory investigation of characteristics of various fuels and for research on combustion in turbulent flames is discussed.

  5. MASS SPECTROMETRIC ANALYSIS FOR THE IDENTIFICATION OF THUNNUS GENUS FOUR SPECIES

    Directory of Open Access Journals (Sweden)

    T. Pepe

    2011-01-01

    Full Text Available An accurate identification of similar fish species is necessary to prevent illegal substitution and is imposed by labeling regulations in UE countries (1. The genus Thunnus comprises many species of different quality and commercial value. The increasing trade of fish preparations of the species included in this genus and the consequent loss of the external anatomical and morphological features enables fraudulent substitutions. This study reports data relating to the proteomic analysis of four tuna species (T. thynnus, T. alalunga, T. albacares, T. obesus. Sarcoplasmic proteins were studied by mono and two dimensional electrophoresis. The most significant proteins for the characterization of the species were analyzed by mass spectrometric techniques. As reported in a previous study (2, an accurate identification of the species seems possible, owing to the polymorphism displayed by the species of the Thunnus genus.

  6. Mass Spectrometric Calibration of Controlled Fluoroform Leak Rate Devices Technique and Uncertainty Analysis

    CERN Document Server

    Balsley, S D; Laduca, C A

    2003-01-01

    Controlled leak rate devices of fluoroform on the order of 10 sup - sup 8 atm centre dot cc sec sup - sup 1 at 25 C are used to calibrate QC-1 War Reserve neutron tube exhaust stations for leak detection sensitivity. Close-out calibration of these tritium-contaminated devices is provided by the Gas Dynamics and Mass Spectrometry Laboratory, Organization 14406, which is a tritium analytical facility. The mass spectrometric technique used for the measurement is discussed, as is the first principals calculation (pressure, volume, temperature and time). The uncertainty of the measurement is largely driven by contributing factors in the determination of P, V and T. The expanded uncertainty of the leak rate measurement is shown to be 4.42%, with a coverage factor of 3 (k=3).

  7. Molecular beam mass spectrometric sampling of minor species from coal dust-air flames

    International Nuclear Information System (INIS)

    It has been demonstrated that unaugmented, unconfined, premixed coal dust-air flames can be stabilized on small conical or flat, Meeker type burners. Since these flames are laminar, they can be used to study the kinetics of various processes in coal combustion and related areas such as understanding mechanisms of fireside corrosion and of flame and explosive inhibition. Some of the current work with these flames is directed toward identification and measurement of minor alkali metal and other species responsible for fireside corrosion. In order to make these measurements, molecular beam mass spectrometric sampling techniques have been adpated for use with these heterogeneous flames. In this paper, the equipment and techniques used are reviewed and some preliminary results presented

  8. Separation and estimation of 229Th and 233U by alpha and gamma ray spectrometric technique

    International Nuclear Information System (INIS)

    The individual estimation of 233U and 229Th in a plancheted source made out of liquid sample were done by using an alpha and γ-ray spectrometric techniques. Estimation of 229Th in the plancheted source was done by γ-ray spectrometry and 233U by alpha spectrometry after subtracting the estimated amount of 229Th. In spite of the same alpha energy of 4.8 MeV, the individual estimation of 233U and 229Th based on present technique is superior to conventional techniques and important in the 232Th-233U fuel reprocessing cycle of AHWR and ADSs. The activity of 229Th was also radiochemically separated from its parent activity of 233U by using an ion exchange resin and the purity was checked by the above mentioned technique. (author)

  9. New fortran computer programs to acquire and process isotopic mass spectrometric data

    International Nuclear Information System (INIS)

    This report describes in some detail the operation of newly written programs that acquire and process isotopic mass spectrometric data. Both functional and overall design aspects are addressed. The three basic program units - file manipulation, data acquisition, and data processing - are discussed in turn. Step-by-step instructions are included where appropriate, and each subsection is described in enough detail to give a clear picture of its function. Organization of the file structure, which is central to the entire concept, is extensively discussed with the help of numerous tables. Appendices contain flow charts and definitions of variables to help a programmer unfamiliar with the programs to alter them with a minimum of lost time. 12 figures, 17 tables

  10. Mass spectrometric identification of proteins and characterization of their post-translational modifications in proteome analysis

    DEFF Research Database (Denmark)

    Roepstorff, P; Larsen, Martin Røssel

    2001-01-01

    more than 425.000 protein sequences. However, the cellular functions are determined by the set of proteins expressed in the cell--the proteome. Two-dimensional gel electrophoresis, mass spectrometry and bioinformatics have become important tools in correlating the proteome with the genome. The current...... dominant strategies for identification of proteins from gels based on peptide mass spectrometric fingerprinting and partial sequencing by mass spectrometry are described. After identification of the proteins the next challenge in proteome analysis is characterization of their post-translational...... modifications. The general problems associated with characterization of these directly from gel separated proteins are described and the current state of art for the determination of phosphorylation, glycosylation and proteolytic processing is illustrated....

  11. A single detector spectrometric portal monitoring concept solving the problems of 'innocent alarms'

    International Nuclear Information System (INIS)

    In order to overcome the problems of 'innocent alarms' due to naturally occurring radioactive material (NORM) in vehicle monitoring and to medical isotopes in pedestrian monitoring, a new technology has been developed in the last few years, based on gamma spectrometry. The US Domestic Nuclear Detection Office (DNDO) has started a new approach to dynamic primary screening of vehicles, namely, advanced spectrometric portals (ASPs) based on multiple NaI scintillation or HPGe detectors. Complex and expensive instruments with up to 14 large volume NaI or HPGe detectors have been built and are presently being tested by DNDO. Up to now, it seems that these ASPs cannot meet the goal of detecting HEU masked by NORM 95% of the time. Even if this could be achieved, the approach is extremely expensive. The proposed new concept is based on a single detector spectrometric portal monitor (SRPM) with one large NaI crystal for dynamic primary screening of pedestrians, luggage, parcels, mail, etc., with immediate identification of innocent alarms. In addition, the SRPM can be used for secondary screening of vehicles in static mode after an alarm is triggered by a conventional plastic scintillator radiation portal monitor. After identification by the SRPM, the radiation source can be quickly localized with a highly sensitive gamma or neutron search detector, faster and easier as compared to a conventional radioisotope identifier device. One SRPM can serve several primary vehicle lanes for secondary inspection. This makes it even more economic. The paper describes test results obtained with a new SRPM, the SPIR IDENT, developed by SynOdys, France. Extensive testing, partly in cooperation with the IAEA, indicates that this instrument can meet the requirements of the IAEA, the International Electrotechnical Commission (IEC) and the American National Standards Institute (ANSI) for dynamic pedestrian monitoring as well as the IEC and ANSI requirements for static vehicle monitoring in

  12. GNU polyxmass: a software framework for mass spectrometric simulations of linear (bio-polymeric analytes

    Directory of Open Access Journals (Sweden)

    Rusconi Filippo

    2006-04-01

    Full Text Available Abstract Background Nowadays, a variety of (bio-polymers can be analyzed by mass spectrometry. The detailed interpretation of the spectra requires a huge number of "hypothesis cycles", comprising the following three actions 1 put forth a structural hypothesis, 2 test it, 3 (invalidate it. This time-consuming and painstaking data scrutiny is alleviated by using specialized software tools. However, all the software tools available to date are polymer chemistry-specific. This imposes a heavy overhead to researchers who do mass spectrometry on a variety of (bio-polymers, as each polymer type will require a different software tool to perform data simulations and analyses. We developed a software to address the lack of an integrated software framework able to deal with different polymer chemistries. Results The GNU polyxmass software framework performs common (bio-chemical simulations–along with simultaneous mass spectrometric calculations–for any kind of linear bio-polymeric analyte (DNA, RNA, saccharides or proteins. The framework is organized into three modules, all accessible from one single binary program. The modules let the user to 1 define brand new polymer chemistries, 2 perform quick mass calculations using a desktop calculator paradigm, 3 graphically edit polymer sequences and perform (bio-chemical/mass spectrometric simulations. Any aspect of the mass calculations, polymer chemistry reactions or graphical polymer sequence editing is configurable. Conclusion The scientist who uses mass spectrometry to characterize (bio-polymeric analytes of different chemistries is provided with a single software framework for his data prediction/analysis needs, whatever the polymer chemistry being involved.

  13. FITPix COMBO—Timepix detector with integrated analog signal spectrometric readout

    Science.gov (United States)

    Holik, M.; Kraus, V.; Georgiev, V.; Granja, C.

    2016-02-01

    The hybrid semiconductor pixel detector Timepix has proven a powerful tool in radiation detection and imaging. Energy loss and directional sensitivity as well as particle type resolving power are possible by high resolution particle tracking and per-pixel energy and quantum-counting capability. The spectrometric resolving power of the detector can be further enhanced by analyzing the analog signal of the detector common sensor electrode (also called back-side pulse). In this work we present a new compact readout interface, based on the FITPix readout architecture, extended with integrated analog electronics for the detector's common sensor signal. Integrating simultaneous operation of the digital per-pixel information with the common sensor (called also back-side electrode) analog pulse processing circuitry into one device enhances the detector capabilities and opens new applications. Thanks to noise suppression and built-in electromagnetic interference shielding the common hardware platform enables parallel analog signal spectroscopy on the back side pulse signal with full operation and read-out of the pixelated digital part, the noise level is 600 keV and spectrometric resolution around 100 keV for 5.5 MeV alpha particles. Self-triggering is implemented with delay of few tens of ns making use of adjustable low-energy threshold of the particle analog signal amplitude. The digital pixelated full frame can be thus triggered and recorded together with the common sensor analog signal. The waveform, which is sampled with frequency 100 MHz, can be recorded in adjustable time window including time prior to the trigger level. An integrated software tool provides control, on-line display and read-out of both analog and digital channels. Both the pixelated digital record and the analog waveform are synchronized and written out by common time stamp.

  14. FITPix COMBO—Timepix detector with integrated analog signal spectrometric readout

    International Nuclear Information System (INIS)

    The hybrid semiconductor pixel detector Timepix has proven a powerful tool in radiation detection and imaging. Energy loss and directional sensitivity as well as particle type resolving power are possible by high resolution particle tracking and per-pixel energy and quantum-counting capability. The spectrometric resolving power of the detector can be further enhanced by analyzing the analog signal of the detector common sensor electrode (also called back-side pulse). In this work we present a new compact readout interface, based on the FITPix readout architecture, extended with integrated analog electronics for the detector's common sensor signal. Integrating simultaneous operation of the digital per-pixel information with the common sensor (called also back-side electrode) analog pulse processing circuitry into one device enhances the detector capabilities and opens new applications. Thanks to noise suppression and built-in electromagnetic interference shielding the common hardware platform enables parallel analog signal spectroscopy on the back side pulse signal with full operation and read-out of the pixelated digital part, the noise level is 600 keV and spectrometric resolution around 100 keV for 5.5 MeV alpha particles. Self-triggering is implemented with delay of few tens of ns making use of adjustable low-energy threshold of the particle analog signal amplitude. The digital pixelated full frame can be thus triggered and recorded together with the common sensor analog signal. The waveform, which is sampled with frequency 100 MHz, can be recorded in adjustable time window including time prior to the trigger level. An integrated software tool provides control, on-line display and read-out of both analog and digital channels. Both the pixelated digital record and the analog waveform are synchronized and written out by common time stamp

  15. Uranium prospection methods illustrated with examples

    International Nuclear Information System (INIS)

    Uranium exploration methods are briefly reviewed: aerial (radiometric, spectrometric), surface (mapping, radiometric, geophysical, geochemical), sub-surface (well logging, boring) and mining methods in the different steps of a mine project: preliminary studies, general prospecting, detailed prospecting deposit area and deposit estimation. Choice of methods depends strongly on geographic and geologic environment. Three examples are given concerning: an intragranitic deposit Limousin (France), a deposit spatially related to a discordance Athabasca (Canada) and a sedimentary deposit Manyingee (Western Australia)

  16. Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

    Institute of Scientific and Technical Information of China (English)

    Petr Lacina; Ludmila Mravcová; Milada Vávrová

    2013-01-01

    Pharmaceutical residues have become tightly controlled environmental contaminants in recent years,due to their increasing concentration in environmental components.This is mainly caused by their high level of production and everyday consumption.Therefore there is a need to apply new and sufficiently sensitive analytical methods,which can detect the presence of these contaminants even in very low concentrations.This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues,mainly from the group of non-steroidal anti-iaffammatory drugs (salicylic acid,acetylsalicylic acid,clofibric acid,ibuprofen,acetaminophen,caffeine,naproxen,mefenamic acid,ketoprofen,and dicofenac),in wastewaters and surface waters.This analytical method is based on solid phase extraction,derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GCxGC-TOF MS).Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix.The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice,Czech Republic.The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.

  17. Integrated Post-Experiment Monoisotopic Mass Refinement: An Integrated Approach to Accurately Assign Monoisotopic Precursor Masses to Tandem Mass Spectrometric Data

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Hee-Jung; Purvine, Samuel O.; Kim, Hokeun; Petyuk, Vladislav A.; Hyung, Seok-Won; Monroe, Matthew E.; Mun, Dong-Gi; Kim, Kyong-Chul; Park, Jong-Moon; Kim, Su-Jin; Tolic, Nikola; Slysz, Gordon W.; Moore, Ronald J.; Zhao, Rui; Adkins, Joshua N.; Anderson, Gordon A.; Lee, Hookeun; Camp, David G.; Yu, Myeong-Hee; Smith, Richard D.; Lee, Sang-Won

    2010-10-15

    Accurate assignment of monoisotopic precursor masses to tandem mass spectrometric (MS/MS) data is a fundamental and critically important step for successful peptide identifications in mass spectrometry based proteomics. Here we describe an integrated approach that combines three previously reported methods of treating MS/MS data for precursor mass refinement. This combined method, “integrated Post-Experiment Monoisotopic Mass Refinement” (iPE MMR), integrates steps: 1) generation of refined MS/MS data by DeconMSn, 2) additional refinement of the resultant MS/MS data by a modified version of PE-MMR, and 3) elimination of systematic errors of precursor masses using DtaRefinery. iPE-MMR is the first method that utilizes all MS information from multiple MS scans of a precursor ion and multiple charge states of it in an MS scan to determine precursor mass. By combining the synergistic features of each of method, iPE MMR increases sensitivity in peptide identification and provides increased accuracy when applied to complex high-throughput proteomics data. iPE MMR also allows incorporating additional data processing step(s) or skipping step(s), if necessary, to enable new developments or applications of the tools, as each step of iPE MMR produces output data in a common and conventional format used in proteomics data processing.

  18. In situ gamma-ray spectrometric analysis of radionuclide distributions at a commercial shallow land burial site

    International Nuclear Information System (INIS)

    Gamma-ray spectrometric analysis conducted at the Maxey Flats, Kentucky (USA) shallow land burial site confirmed that the waste radionuclides have been retained largely within the restricted area of the burial site. Concentrations of 137Cs and 60Co were comparable with those originating from global fallout and lower than concentrations measured in several other areas having similar rainfall. In-situ spectrometric analyses, corroborated by soil sample and vegetation analyses, indicate that the site has influenced 60Co levels slightly in the west drainage channel, but 137Cs did not originate from the site. Concentrations of 60Co, 90Sr and 137Cs determined in subsurface soils by well logging techniques confirmed that subsurface migration of waste-derived radionuclides to points outside the restricted area has not been a significant source of contamination of the environs adjacent to the site. 8 references, 8 figures

  19. Determination of fission cross-section and absolute fission yields using track-cum gamma-ray spectrometric technique

    International Nuclear Information System (INIS)

    The fission cross-section of 233Pa(2nth, f) using fission track technique has been determined for the first time using thermal neutron flux of the reactor APSARA. This is important from the point of view of advance heavy water reactor (AHWR), which is to be described. On the other hand, the yields of fission products in the fast neutron induced fission of minor actinides are important from the point accelerator driven sub critical system (ADSS). In view of that, absolute yields of fission products in the fast neutron induced fission of 238U, 237Np, 238,240Pu, 243Am and 244Cm have been determined using the fission track-cum gamma-ray spectrometric technique. The total number of fission occurring in the target was estimated by track technique, whereas the activities of the fission products have been determined using gamma-ray spectrometric technique. Detailed procedure and its importance are to be discussed. (author)

  20. Mobile computerized gamma-ray and x-ray spectrometric-analysis and data-processing system

    International Nuclear Information System (INIS)

    A mobile, computerized gamma-ray and x-ray spectrometric-analysis and date-processing system has been designed, assembled, and evaluated. The system consists of a specially constructed vehicle, multichannel analyzer, and data-processing equipment mounted in the vehicle and germanium detectors that can be moved to locations external to the vehicle for use. Applications of the system include nuclear-material safeguards measurement, in situ radionuclide analysis, activation analysis, and research support

  1. Study of the spectrometric performances of monolithic CdTe CdZnTe gamma ray detectors

    OpenAIRE

    Gros D'Aillon, Eric

    2005-01-01

    Pixelated monolithic CdTe / CdZnTe semiconductor gamma ray detectors are brought to replace scintillation detectors for medical applications, notably for single photon emission computed tomography (SPECT). In addition to compactness, they present better spectrometric performances: energy resolution, detection efficiency, and spatial resolution. Moreover, the photons depth of interaction in the crystal can be measured. This work aimed in studying experimentally and by simulation the correlatio...

  2. Impact of the Pixel Pitch of the Timepix Chip Integrated to the GAMPIX Gamma Camera for Spectrometric and Imaging Performances

    International Nuclear Information System (INIS)

    Spatial localization and identification of radioactive sources is a main issue interesting Homeland Security. Gamma imaging allows reaching this need. A new gamma camera, GAMPIX, has been designed by the French Atomic Energy Commission (CEA). GAMPIX enables spatial localization of hot spots on a large energy range. Sensitivity, portability (2 kg) and ergonomics were improved in comparison with previous industrial systems. The detection system is based on the 1.4 cm side Timepix pixelated readout chip developed by CERN and hybridized to a 1 mm thick CdTe substrate. Pixel size of the Timepix chip is 55 μm or 110 μm. Ongoing developments concern the addition of a spectrometric capability to the existing system. The challenge is the optimization of spectrometric performances while maintaining imaging performances. Our work intends to assess the impact of pixel pitch by means of simulations and experimental validation. A large range of pixel pitch and energies were tested by MCNPX simulations. Fluorescence impact depending on pixel pitch was demonstrated. Pixel pitch impact on imaging performances was also studied. The purpose is to preserve the angular resolution of the GAMPIX gamma camera, i.e., the ability to separate radioactive sources spatially close. Energy calibration of Timepix detectors is crucial for the optimization of spectrometric performances. The small pixel size compared to the substrate thickness induces charge depositions in several pixels, called clusters, and the shift between spectra due to different cluster sizes degrades the energy resolution. The energy calibration of our Timepix detectors was carried out in the SOLEX tunable monochromatic X-ray source (CEA). Our developments show that the replacement of the 55 μm pixelated Timepix chip currently used in the GAMPIX gamma camera by a 110 μm pixel pitch would lead to a significant improvement in terms of spectrometric performances without degrading imaging abilities. (author)

  3. Airborne gamma-ray spectrometric anomaly characteristics and prospecting model for quaternary salt lake type potash deposit

    International Nuclear Information System (INIS)

    On the basis of the airborne gamma-ray spectrometric data, this paper briefly discusses partial scientific research achievements related to prospecting for potash and the establishment of prospecting model for Quaternary salt lake type potash deposit, and furthermore through the analysis on Bieletan and Mahai Potash deposits, it shows that airborne gamma-ray spectrometry is certainly of evident effect in prospecting for Quaternary salt lake type potash deposit

  4. Parallel Workflow for High-Throughput (>1,000 Samples/Day) Quantitative Analysis of Human Insulin-Like Growth Factor 1 Using Mass Spectrometric Immunoassay

    Science.gov (United States)

    Oran, Paul E.; Trenchevska, Olgica; Nedelkov, Dobrin; Borges, Chad R.; Schaab, Matthew R.; Rehder, Douglas S.; Jarvis, Jason W.; Sherma, Nisha D.; Shen, Luhui; Krastins, Bryan; Lopez, Mary F.; Schwenke, Dawn C.; Reaven, Peter D.; Nelson, Randall W.

    2014-01-01

    Insulin-like growth factor 1 (IGF1) is an important biomarker for the management of growth hormone disorders. Recently there has been rising interest in deploying mass spectrometric (MS) methods of detection for measuring IGF1. However, widespread clinical adoption of any MS-based IGF1 assay will require increased throughput and speed to justify the costs of analyses, and robust industrial platforms that are reproducible across laboratories. Presented here is an MS-based quantitative IGF1 assay with performance rating of >1,000 samples/day, and a capability of quantifying IGF1 point mutations and posttranslational modifications. The throughput of the IGF1 mass spectrometric immunoassay (MSIA) benefited from a simplified sample preparation step, IGF1 immunocapture in a tip format, and high-throughput MALDI-TOF MS analysis. The Limit of Detection and Limit of Quantification of the resulting assay were 1.5 μg/L and 5 μg/L, respectively, with intra- and inter-assay precision CVs of less than 10%, and good linearity and recovery characteristics. The IGF1 MSIA was benchmarked against commercially available IGF1 ELISA via Bland-Altman method comparison test, resulting in a slight positive bias of 16%. The IGF1 MSIA was employed in an optimized parallel workflow utilizing two pipetting robots and MALDI-TOF-MS instruments synced into one-hour phases of sample preparation, extraction and MSIA pipette tip elution, MS data collection, and data processing. Using this workflow, high-throughput IGF1 quantification of 1,054 human samples was achieved in approximately 9 hours. This rate of assaying is a significant improvement over existing MS-based IGF1 assays, and is on par with that of the enzyme-based immunoassays. Furthermore, a mutation was detected in ∼1% of the samples (SNP: rs17884626, creating an A→T substitution at position 67 of the IGF1), demonstrating the capability of IGF1 MSIA to detect point mutations and posttranslational modifications. PMID:24664114

  5. Parallel workflow for high-throughput (>1,000 samples/day quantitative analysis of human insulin-like growth factor 1 using mass spectrometric immunoassay.

    Directory of Open Access Journals (Sweden)

    Paul E Oran

    Full Text Available Insulin-like growth factor 1 (IGF1 is an important biomarker for the management of growth hormone disorders. Recently there has been rising interest in deploying mass spectrometric (MS methods of detection for measuring IGF1. However, widespread clinical adoption of any MS-based IGF1 assay will require increased throughput and speed to justify the costs of analyses, and robust industrial platforms that are reproducible across laboratories. Presented here is an MS-based quantitative IGF1 assay with performance rating of >1,000 samples/day, and a capability of quantifying IGF1 point mutations and posttranslational modifications. The throughput of the IGF1 mass spectrometric immunoassay (MSIA benefited from a simplified sample preparation step, IGF1 immunocapture in a tip format, and high-throughput MALDI-TOF MS analysis. The Limit of Detection and Limit of Quantification of the resulting assay were 1.5 μg/L and 5 μg/L, respectively, with intra- and inter-assay precision CVs of less than 10%, and good linearity and recovery characteristics. The IGF1 MSIA was benchmarked against commercially available IGF1 ELISA via Bland-Altman method comparison test, resulting in a slight positive bias of 16%. The IGF1 MSIA was employed in an optimized parallel workflow utilizing two pipetting robots and MALDI-TOF-MS instruments synced into one-hour phases of sample preparation, extraction and MSIA pipette tip elution, MS data collection, and data processing. Using this workflow, high-throughput IGF1 quantification of 1,054 human samples was achieved in approximately 9 hours. This rate of assaying is a significant improvement over existing MS-based IGF1 assays, and is on par with that of the enzyme-based immunoassays. Furthermore, a mutation was detected in ∼1% of the samples (SNP: rs17884626, creating an A→T substitution at position 67 of the IGF1, demonstrating the capability of IGF1 MSIA to detect point mutations and posttranslational modifications.

  6. Identification of Polish cochineal (Porphyrophora polonica L.) in historical textiles by high-performance liquid chromatography coupled with spectrophotometric and tandem mass spectrometric detection.

    Science.gov (United States)

    Lech, Katarzyna; Jarosz, Maciej

    2016-05-01

    The present work reports a method for identification of Polish cochineal (Porphyrophora polonica L.) in historical fabrics by the use of high-performance liquid chromatography coupled with diode array and tandem mass spectrometric detection with electrospray ionization (HPLC-DAD-ESI MS/MS). This hyphened technique allows detection and identification of 16 new minor colorants present in the discussed scale insect (including two previously observed by Wouters and Verhecken (Ann Soc Entomol Fr. 1989;25:393-410), but specified only as compounds of unknown structures) that do not occur (e.g., in American cochineal). The MS/MS experiments, complemented with UV-VIS data, enable identification of mono- and di-, C- and O-hexosides of kermesic and flavokermesic acids or their derivatives. The present paper introduces a fingerprint of color compounds present in Polish cochineal and defines them, particularly pp6 (ppI, O-hexoside of flavokermesic acid), as its markers allow distinguishing of Polish-cochineal reds from the American ones. Usefulness of the selected set of markers for identification of Polish cochineal has been demonstrated in the examination of textiles from the collection of the National Museum in Warsaw using the multiple reaction monitoring (MRM) method, originally elaborated on the basis of this study. PMID:26935929

  7. Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometric Analysis of the Recombinant Human Macrophage Colony Stimulating Factor Beta and Derivatives

    International Nuclear Information System (INIS)

    The potential of electrospray ionization (ESI) Fourier transform ion cyclotron mass spectrometry (FTICR-MS) to assist in the structural characterization of monomeric and dimeric derivatives of the macrophage colony stimulating factor B (rhM-CSF B) was assessed. Mass spectrometric analysis of the 49 kDa protein required the use of sustained off-resonance irradiation (SORI) in-trap cleanup to reduce adduction. High resolution mass spectra were acquired for a fully reduced and a fully S-cyanylated monomeric derivative (∼25 kDa). Mass accuracy for monomeric derivatives was better than 5 ppm, after applying a new calibration method (i.e., DeCAL) which eliminates space charge effects upon high accuracy mass measurements. This high mass accuracy allowed the direct determination of the exact number of incorporated cyanyl groups. Collisionally induced dissociation using SORI yielded b- and y-fragment ions within the N- and C-terminal regions for the monomeric derivatives, but obtaining information on other regions required proteolytic digestion, or potentially the use of alternative dissociation methods

  8. A Simple and Effective Mass Spectrometric Approach to Identify the Adulteration of the Mediterranean Diet Component Extra-Virgin Olive Oil with Corn Oil

    Directory of Open Access Journals (Sweden)

    Francesco Di Girolamo

    2015-09-01

    Full Text Available Extra virgin olive oil (EVOO with its nutraceutical characteristics substantially contributes as a major nutrient to the health benefit of the Mediterranean diet. Unfortunately, the adulteration of EVOO with less expensive oils (e.g., peanut and corn oils, has become one of the biggest source of agricultural fraud in the European Union, with important health implications for consumers, mainly due to the introduction of seed oil-derived allergens causing, especially in children, severe food allergy phenomena. In this regard, revealing adulterations of EVOO is of fundamental importance for health care and prevention reasons, especially in children. To this aim, effective analytical methods to assess EVOO purity are necessary. Here, we propose a simple, rapid, robust and very sensitive method for non-specialized mass spectrometric laboratory, based on the matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS coupled to unsupervised hierarchical clustering (UHC, principal component (PCA and Pearson’s correlation analyses, to reveal corn oil (CO adulterations in EVOO at very low levels (down to 0.5%.

  9. Gamma-spectrometric module based on HPGe detector for radiation portal monitors

    Directory of Open Access Journals (Sweden)

    Kondratjev Vladimir

    2015-01-01

    Full Text Available The appearance of small-sized and powerful enough electric cryocoolers of various types on the market, has opened the perspective of HPGe detectors application, cooled by such coolers, in radiation portal monitors. The first results of a spectrometric module based on HPGe detector with relative efficiency of 45% cooled by a Stirling-cycle cryocooler, are presented. The spectrometer has provided energy resolutions of less than 0.95 keV and 1.95 keV at energies of 122 keV and 1332 keV, respectively. The deterioration of the energy resolution of HPGe detector cooled by electric cryocooler in comparison to the resolution with liquid nitrogen cooling was about 8% at the energy of 1332 keV. With the use of activated filters to suppress pulses produced by the mechanical vibrations, the energy resolution of the spectrometer was 0.8 keV and 1.8 keV, respectively, however, the detector relative efficiency at the energy of 1332 keV has dropped to 39 %.

  10. Uranium remobilization and migration evaluation through aerial spectrometric gamma technique in Syrian Desert (Area-1), Syria.

    Science.gov (United States)

    Asfahani, J; Al-Hent, R; Aissa, M

    2016-01-01

    Uranium remobilization and migration in the Syrian Desert (Area-1) has been evaluated through analyzing the data of aerial spectrometric gamma technique and examining different radioactive geophysical approaches. The ten geological units identified on the already established scored map have been well characterized through analyzing their contents of eU, eTh, and K%, and studying the mutual relationships between those elements and their ratios. This is done in order to define the regional variation trends of the uranium migration in Area-1, and to evaluate the degree of uranium remobilization. The uranium potential in the studied Area-1 has been explained by applying and analyzing two prospecting indicators of the uranium favorability index UI and alteration-F. It was demonstrated that uranium remobilization took place in all the described lithological units, but to different degrees. The uranium migration and its haloes redistributions have been explained by establishing different plausible geological model interpretations. Several localities such as wadi Ratka are found to be favorable possible traps for uranium accumulation, which necessitate more further detailed uranium exploration. PMID:26629682

  11. Mass spectrometric survey of peptides in cephalopods with an emphasis on the FMRFamide-related peptides.

    Science.gov (United States)

    Sweedler, J V; Li, L; Floyd, P; Gilly, W

    2000-12-01

    A matrix-assisted laser desorption/ionization (MALDI) mass spectrometric (MS) survey of the major peptides in the stellar, fin and pallial nerves and the posterior chromatophore lobe of the cephalopods Sepia officinalis, Loligo opalescens and Dosidicus gigas has been performed. Although a large number of putative peptides are distinct among the three species, several molecular masses are conserved. In addition to peptides, characterization of the lipid content of the nerves is reported, and these lipid peaks account for many of the lower molecular masses observed. One conserved set of peaks corresponds to the FMRFamide-related peptides (FRPs). The Loligo opalescens FMRFa gene has been sequenced. It encodes a 331 amino acid residue prohormone that is processed into 14 FRPs, which are both predicted by the nucleotide sequence and confirmed by MALDI MS. The FRPs predicted by this gene (FMRFa, FLRFa/FIRFa and ALSGDAFLRFa) are observed in all three species, indicating that members of this peptide family are highly conserved across cephalopods. PMID:11060217

  12. Determination of ractopamine in pig hair using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Wu, Junlin; Liu, Xiaoyun; Peng, Yunping

    2014-01-01

    A quantitative analytical procedure for the determination of ractopamine in pig hair has been developed and validated. The hair samples were washed and incubated at 75°C with isoxuprine and hair extraction buffer. The drug present was quantified using mixed solid-phase extraction and liquid chromatography with tandem mass spectrometric detection. The limit of quantization (LOQ) was 10pg/mg and the intra-day precision at 25pg/mg and 750pg/mg was 0.49% and 2.8% respectively. Inter-day precision was 0.88% and 3.52% at the same concentrations. The hair extraction percentage recovery at 25pg/mg and 50ng/mL was 99.47% and 103.83% respectively. The extraction percentage recovery at 25pg/mg and 50ng/mg was 93.52% and 100.26% respectively. Our results showed that ractopamine residues persist in hair in 24days of withdrawal and also showed the possibility to test ractopamine from pig hair samples. PMID:24548851

  13. Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina)

    2015-05-22

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

  14. Combined chromatographic and mass spectrometric toolbox for fingerprinting migration from PET tray during microwave heating.

    Science.gov (United States)

    Alin, Jonas; Hakkarainen, Minna

    2013-02-13

    A combined chromatographic and mass spectrometric toolbox was utilized to determine the interactions between poly(ethylene terephthalate) (PET) food packaging and different food simulants during microwave heating. Overall and specific migration was determined by combining weight loss measurements with gas chromatography-mass spectrometry (GC-MS) and electrospray ionization mass spectrometry (ESI-MS). This allowed mapping of low molecular weight migrants in the molecular range up to 2000 g/mol. Microwave heating caused significantly faster migration of cyclic oligomers into ethanol and isooctane as compared to migration during conventional heating at the same temperature. This effect was more significant at lower temperature at which diffusion rates are generally lower. It was also shown that transesterification took place between PET and ethanol during microwave heating, leading to formation of diethyl terephthalate. The detected migrants included cyclic oligomers from dimer to hexamer, in most cases containing extra ethylene glycol units, and oxidized Irgafos 168. ESI-MS combined with CID MS-MS was an excellent tool for structural interpretation of the nonvolatile compounds migrating to the food simulants. The overall migration was below the overall migration limit of 10 mg/dm(2) set by the European commission after 4 h of microwave heating at 100 °C in all studied food simulants. PMID:23343184

  15. Gamma spectrometrical analyses of annual deposition samples collected in Romania in 1987-1989

    International Nuclear Information System (INIS)

    The dynamics of artificial radionuclide concentrations in deposition samples in the years 1987-1989 is presented in this paper. High resolution gamma spectrometrical analyses have been performed on wet and dry deposition samples from the following stations of the National Environmental Radioactivity Surveillance Network: Cluj-Napoca, Satu-Mare, Constanta, Ceahlau-Tosca, lasi and Craiova. In order to determine small concentrations of low level artificial radionuclides (having an appropriate half life) yearly samples obtained by cumulating daily samples were measured. The following gamma emitting radionuclides were identified in these samples: 106Ru, 110mAg, 125Sb, 134Cs, 137Cs, 144Ce. It can be seen that the level of radionuclide activities in deposition samples at any time is dependent on the 'initial' deposition of May 1986. An environmental half life of 137Cs in deposition can be assessed. For a particular case the evolution during 1987-1989 of 137Cs and 7Be specific activities in monthly samples is also presented. (author)

  16. Method-MS, final report 2010

    DEFF Research Database (Denmark)

    Skipperud, Lindis; Popic, Jelena M.; Roos, Per;

    (AMS) have shown several advantages compared to traditional methods when measuring long-lived radionuclides. Mass spectrometric methods for determination of very low concentrations of elemental isotopes, and thereby isotopic ratios, have been developed using a variety of ion sources. Although primarily...... applied to the determination of the lighter stable element isotopes and radioactive isotopes in geological studies, the techniques can equally well be applied to the measurement of activity concentrations of long-lived low-level radionuclides in various samples using “isotope dilution” methods such as...... those applied in inductively coupled plasma mass spectrometry (ICP-MS). Due to the low specific activity of long-lived radionuclides, many of these are more conveniently detected using mass spectrometric techniques. Mass spectrometry also enables the individual determination of Pu-239 and Pu-240, which...

  17. Application of high-performance liquid chromatography combined with ultra-sensitive thermal lens spectrometric detection for simultaneous biliverdin and bilirubin assessment at trace levels in human serum.

    Science.gov (United States)

    Martelanc, Mitja; Žiberna, Lovro; Passamonti, Sabina; Franko, Mladen

    2016-07-01

    We present the applicability of a new ultra-sensitive analytical method for the simultaneous determination of biliverdin and bilirubin in human serum. The method comprises isocratic reversed-phase (RP) C18 high-performance liquid chromatography (HPLC) and thermal lens spectrometric detection (TLS) based on excitation by a krypton laser emission line at 407nm. This method enables the separation of IX-α biliverdin and IX-α bilirubin in 11min with limit of detection (LOD) and limit of quantitation (LOQ) for biliverdin of 1.2nM and 3nM, and 1nM and 2.8nM for bilirubin, respectively. In addition, a step-gradient elution was set up, by changing the mobile phase composition, in order to further enhance the sensitivity for bilirubin determination with LOD and LOQ of 0.5nM and 1.5nM, respectively. In parallel, an isocratic HPLC-DAD method was developed for benchmarking against HPLC-TLS methods. The LOD and LOQ for biliverdin were 6nM and 18nM, and 2.5nM and 8nM for bilirubin, respectively. Additionally, both isocratic methods were applied for measuring biliverdin and free bilirubin in human serum samples (from 2 male and 2 female healthy donors). Combining isocratic HPLC method with TLS detector was crucial for first ever biliverdin determination in serum together with simultaneous free bilirubin determination. We showed for the first time the concentration ratio of free bilirubin versus unbound biliverdin in human serum samples. PMID:27154653

  18. Flame atomic absorption spectrometric determination of cadmium(II) and lead(II) after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493

    International Nuclear Information System (INIS)

    An enrichment procedure for cadmium and lead after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493 has been established prior to their flame atomic absorption spectrometric determinations. The analytical parameters including pH, amounts of dibenzyldithiocarbamate, sample volume, etc., were investigated. The effects of alkaline and earth alkaline ions and some metal ions on the retentions of analytes on Dowex Optipore V-493 resin were examined. Under the optimized conditions, the detection limits (3s, n = 21) for cadmium and lead were 0.43 μg L-1 and 0.65 μg L-1, respectively. The relative standard deviation (R.S.D.), and the recoveries of standard addition for this method were lower than 5% (n = 11) and 95-102%, respectively. Three standard reference samples (LGC 6010 Hard drinking water, NIST SRM 2711 Montana soil and GBW 07605 Tea) were introduced for accuracy and precision of analytical data. The proposed solid phase extraction system was successfully applied to the analysis of environmental samples

  19. [Determination of nine estrogenic steroids in milk using matrix solid phase dispersion-ultra performance liquid chromatography with mass spectrometric detector].

    Science.gov (United States)

    Liu, Hongcheng; Li, Ning; Lin, Tao; Shao, Jinliang; Li, Qiwan

    2015-11-01

    An analytical method for the multiresidue determination of nine estrogenic steroids in milk was developed by modified matrix solid phase dispersion (MSPD) purification and ultra performance liquid chromatography (UPLC) with mass spectrometric detector (MSD). The sensitivity and accuracy of MSD were better than that of ultraviolet detector. In comparison with traditional mass spectrometry, the merits of MSD were simpler in operation and shorter in starting time (5 min). The results showed that the limits of detection of the compounds with nucleophilic substitution were high in positive ion mode of MSD and were easily affected by environmental conditions. The matrix effects of milk samples reduced from 84%-160% to 80%-121% after MSPD purification. The intraday precision and interday precision of the nine estrogenic steroids were 0.87%-1.78% and 1.82%-3.79%, respectively. The average recoveries were 68.7%-94.7%, and the relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) were 0.5-10 μg/kg. The limits of quantification (LOQ) were 2-20 μg/kg. PMID:26939362

  20. Evaluation of mass spectrometric data using principal component analysis for determination of the effects of organic lakes on protein binder identification.

    Science.gov (United States)

    Hrdlickova Kuckova, Stepanka; Rambouskova, Gabriela; Hynek, Radovan; Cejnar, Pavel; Oltrogge, Doris; Fuchs, Robert

    2015-11-01

    Matrix-assisted laser desorption/ionisation-time of flight (MALDI-TOF) mass spectrometry is commonly used for the identification of proteinaceous binders and their mixtures in artworks. The determination of protein binders is based on a comparison between the m/z values of tryptic peptides in the unknown sample and a reference one (egg, casein, animal glues etc.), but this method has greater potential to study changes due to ageing and the influence of organic/inorganic components on protein identification. However, it is necessary to then carry out statistical evaluation on the obtained data. Before now, it has been complicated to routinely convert the mass spectrometric data into a statistical programme, to extract and match the appropriate peaks. Only several 'homemade' computer programmes without user-friendly interfaces are available for these purposes. In this paper, we would like to present our completely new, publically available, non-commercial software, ms-alone and multiMS-toolbox, for principal component analyses of MALDI-TOF MS data for R software, and their application to the study of the influence of heterogeneous matrices (organic lakes) for protein identification. Using this new software, we determined the main factors that influence the protein analyses of artificially aged model mixtures of organic lakes and fish glue, prepared according to historical recipes that were used for book illumination, using MALDI-TOF peptide mass mapping. PMID:26505772

  1. A mass spectrometric system for analyzing thermal desorption spectra of ion-implanted argon and cesium in tungsten. Ph.D. Thesis

    Science.gov (United States)

    Wood, G. M., Jr.

    1974-01-01

    A mass spectrometric system for determining the characteristics of materials used in instrumental development and aerospace applications was developed. The desorption spectra of cesium that was ion-implanted into polycrystalline tungsten and the effects on the spectra of bombardment of the tungsten by low energy (70 eV) electrons were investigated. Work function changes were measured by the retarding potential diode method. Flash desorption characteristics were observed and gas-reaction mechanisms of the surface of heated metal filaments were studied. Desorption spectra were measured by linearly increasing the sample temperature at a selected rate, the temperature cycling being generated from a ramp-driven dc power supply, with the mass spectrometer tuned to a mass number of interest. Results of the study indicate an anomolous desorption mechanism following an electron bombardment of the sample surface. The enhanced spectra are a function of the post-bombardment time and energy and are suggestive of an increased concentration of cesium atoms, up to 10 or more angstroms below the surface.

  2. Chemical and spectroscopic characterizations, ESI-QTOF mass spectrometric measurements and DFT studies of new complexes of palladium(II) with tryptamine and mefenamic acid

    Science.gov (United States)

    Carvalho, Marcos A.; Arruda, Eduardo G. R.; Profirio, Daniel M.; Gomes, Alexandre F.; Gozzo, Fábio C.; Formiga, André L. B.; Corbi, Pedro P.

    2015-11-01

    New palladium(II) complexes with tryptamine (Pd-tra) and mefenamic acid (Pd-mef) were prepared and characterized by chemical and spectroscopic methods. Elemental, ESI-QTOF mass spectrometric and thermogravimetric analyses of the compounds confirm the composition [PdCl2(tra)2] for Pd-tra and [Pd(mef)2(bipy)] for Pd-mef. Infrared data indicate the coordination of tryptamine to Pd(II) by the nitrogen atom of the amino group, while for mefenamic acid coordination occurs by the oxygen atom of carboxylate group in a monodentate form. The 1H, 13C and {15N,1H} NMR spectroscopic data confirm the nitrogen coordination of the NH2 group of trypatmine to Pd(II) in the Pd-tra complex and also the oxygen coordination of the carboxylate group of mefenamic acid to Pd(II) in the Pd-mef complex. Density functional theory (DFT) studies were applied to determine the difference in energy between the geometric isomers (cis/trans) of Pd-tra and to optimize the structure of the Pd-mef complex. Raman spectroscopic measurements reinforce the nitrogen coordination of tryptamine to Pd(II) in the Pd-tra complex and confirms the presence of the cis-[PdCl2(tra)2] isomer in the solid state. The complexes are insoluble in water.

  3. Single-walled carbon nanotubes coated fibers for solid-phase microextraction and gas chromatography-mass spectrometric determination of pesticides in Tea samples.

    Science.gov (United States)

    Wu, Fang; Lu, Wanping; Chen, Jinghua; Liu, Wei; Zhang, Lan

    2010-08-15

    Using a single-walled carbon nanotubes (SWCNTs) as stationary phase of solid-phase microextraction (SPME) fibers, a simple, low cost and environmentally friendly method for extraction of 13 pesticides in Tea samples has been developed following gas chromatography-mass spectrometric determination. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction and desorption time, extraction temperature, stirring rate, solution pH and ionic strength. Under optimized conditions, the linearity of the developed method was in the range of 0.125-25 ng/mL with correlation coefficients greater than 0.9928 and the limits of detections (LODs) were 0.027-0.23 ng/mL (S/N=3). Meanwhile, the relative standard deviations (RSDs) for five successive measurements with single fiber, fiber-to-fiber, day-to-day were 2.3-13.0, 8.2-14.6 and 4.1-12.5%, respectively, indicating good reproducibility of the proposed method. The fiber had high extraction efficiency for studied pesticides in comparison with commercial poly(dimethylsiloxane) (PDMS) and polyacrylate (PA) fibers and could be used for more than 70 times without decrease of efficiency. The developed method was successfully applied for the analysis of real samples including green Tea, oolong Tea, white Tea, and flower Tea, and the recoveries of the pesticides spiked in these samples ranged from 75.1 to 118.4%. Chlorfenapyr and lambda-cyhalothrin were found in the Tea samples bought randomly from local market. The results demonstrated that the developed SWCNTs-SPME method was a simple, efficient pretreatment and enrichment procedure for pesticides in complex matrices. PMID:20678665

  4. Rapid Mass Spectrometric Analysis of a Novel Fucoidan, Extracted from the Brown Alga Coccophora langsdorfii

    Directory of Open Access Journals (Sweden)

    Stanislav D. Anastyuk

    2014-01-01

    Full Text Available The novel highly sulfated (35% fucoidan fraction Cf2 , which contained, along with fucose, galactose and traces of xylose and uronic acids was purified from the brown alga Coccophora langsdorfii. Its structural features were predominantly determined (in comparison with fragments of known structure by a rapid mass spectrometric investigation of the low-molecular-weight fragments, obtained by “mild” (5 mg/mL and “exhaustive” (maximal concentration autohydrolysis. Tandem matrix-assisted laser desorption/ionization mass spectra (MALDI-TOF/TOFMS of fucooligosaccharides with even degree of polymerization (DP, obtained by “mild” autohydrolysis, were the same as that observed for fucoidan from Fucus evanescens, which have a backbone of alternating (1 → 3- and (1 → 4 linked sulfated at C-2 and sometimes at C-4 of 3-linked α-L-Fucp residues. Fragmentation patterns of oligosaccharides with odd DP indicated sulfation at C-2 and at C-4 of (1 → 3 linked α-L-Fucp residues on the reducing terminus. Minor sulfation at C-3 was also suggested. The “exhaustive” autohydrolysis allowed us to observe the “mixed” oligosaccharides, built up of fucose/xylose and fucose/galactose. Xylose residues were found to occupy both the reducing and nonreducing termini of FucXyl disaccharides. Nonreducing galactose residues as part of GalFuc disaccharides were found to be linked, possibly, by 2-type of linkage to fucose residues and were found to be sulfated, most likely, at position C-2.

  5. Method-MS. Final report

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-05-15

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

  6. Method-MS. Final report

    International Nuclear Information System (INIS)

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

  7. A Sensitive and Robust Ultra HPLC Assay with Tandem Mass Spectrometric Detection for the Quantitation of the PARP Inhibitor Olaparib (AZD2281 in Human Plasma for Pharmacokinetic Application

    Directory of Open Access Journals (Sweden)

    Jeffrey Roth

    2014-06-01

    Full Text Available Olaparib (AZD2281 is an orally active PARP-1 inhibitor, primarily effective against cancers with BRCA1/2 mutations. It is currently in Phase III development and has previously been investigated in numerous clinical trials, both as a single agent and in combination with chemotherapy. Despite this widespread testing, there is only one published method that provides assay details and stability studies for olaparib alone. A more sensitive uHPLC-MS/MS method for the quantification of olaparib in human plasma was developed, increasing the range of quantification at both ends (0.5–50,000 ng/mL compared to previously published methods (10–5,000 ng/mL. The wider range encompasses CMAX levels produced by typical olaparib doses and permits better pharmacokinetic modeling of olaparib elimination. This assay also utilizes a shorter analytical runtime, allowing for more rapid quantification and reduced use of reagents. A liquid-liquid extraction was followed by chromatographic separation on a Waters UPLC® BEH C18 column (2.1 × 50 mm, 1.7 µm and mass spectrometric detection. The mass transitions m/z 435.4→281.1 and m/z 443.2→281.1 were used for olaparib and the internal standard [2H8]-olaparib, respectively. The assay proved to be accurate (<9% deviation and precise (CV < 11%. Stability studies showed that olaparib is stable at room temperature for 24 h. in whole blood, at 4 °C for 24 h post-extraction, at −80 °C in plasma for at least 19 months, and through three freeze-thaw cycles. This method proved to be robust for measuring olaparib levels in clinical samples from a Phase I trial.

  8. Mass spectrometric analysis of laser evaporation products of ceramics of Bi2Sr2CaCu2Ox composition

    International Nuclear Information System (INIS)

    Mass spectrometric analysis is used to study mechanism of laser evaporation of superconducting ceramics of Bi2Sr2CaCu2Ox composition. During evaporation as a result of pulsed laser irradiation of a sample placed in vaccum ions of all metals containing in ceramics and also neutral O2, Ca, Sr, Cu, Bi and metal oxides were detected on yttrium aluminate. Time-of-flight spectra had two peaks corresponding to ion and neutral components. Comparison of neutral components. Comparison of neutral particle rates points to the fact that gas dynamic processes connected with formation of dense gas cloud near the target surface play an important

  9. Chromatographic separation and inductively coupled plasma atomic emission spectrometric determination of the rare earth metals contained in terbium

    International Nuclear Information System (INIS)

    The chromatographic separation of rare earth elements (REEs), prior to inductively coupled plasma atomic emission spectrometric (ICP-AES) measurements, using a column packed with 2-ethylexyl hydrogen 2-ethyl-hexylphosphonate (PC-88A)-loaded polymer resin in order to exclude spectral interferences was examined. A favourable separation of trace amounts of metals (La, Nd and Sm) from a large amount of terbium was achieved simply by elution with dilute hydrochloric acid. Trace lanthanum and neodymium in metallic terbium were determined by separation of the analyte ions from the matrix element followed by ICP-AES analysis. (author). 16 refs.; 5 figs.; 2 tabs

  10. Method

    Directory of Open Access Journals (Sweden)

    Xixin Wang

    2012-01-01

    Full Text Available ZrO2 nanotube arrays were prepared by anodization method in aqueous electrolyte containing (NH42SO4 and NH4F. The morphology and structure of nanotube arrays were characterized through scanning electron microscope, X-ray diffraction, and infrared spectra analysis. The zirconia nanotube arrays were used as catalyst in esterification reaction. The effects of calcination temperature and electrolyte concentration on catalytic esterification activity have been investigated in detail. Experiments indicate that nanotube arrays have highest catalytic activity when the concentration of (NH42SO4 is 1 mol/L, the concentration of NH4F is 1 wt%, and the calcination temperature is 400°C. Esterification reaction yield of as much as 97% could be obtained under optimal conditions.

  11. In Situ Probing of Cholesterol in Astrocytes at the Single Cell Level using Laser Desorption Ionization Mass Spectrometric Imaging with Colloidal Silver

    Energy Technology Data Exchange (ETDEWEB)

    Perdian, D.C.; Cha, Sangwon; Oh, Jisun; Sakaguchi, Donald S.; Yeung, Edward S.; and Lee, Young Jin

    2010-03-18

    Mass spectrometric imaging has been utilized to localize individual astrocytes and to obtain cholesterol populations at the single-cell level in laser desorption ionization (LDI) with colloidal silver. The silver ion adduct of membrane-bound cholesterol was monitored to detect individual cells. Good correlation between mass spectrometric and optical images at different cell densities indicates the ability to perform single-cell studies of cholesterol abundance. The feasibility of quantification is confirmed by the agreement between the LDI-MS ion signals and the results from a traditional enzymatic fluorometric assay. We propose that this approach could be an effective tool to study chemical populations at the cellular level.

  12. Mathematical method for pig iron specific activity determination

    International Nuclear Information System (INIS)

    An original method for pig iron specific activity determination is presented. The mathematical method described is based on the Monte Carlo procedure and is referred to two practical stiuations determined by whether the nature of radionuclide contaminating the pig iron is known or not. Two methods for pig iron specific activity determination, a global and a spectrometric one, are presented, each of them being used in one of the practical situations mentioned above. (author)

  13. Development of destructive methods of burn-up determination and their application on WWER type nuclear fuels

    International Nuclear Information System (INIS)

    Results are described of a cooperation between the Central Institute of Nuclear Research Rossendorf and the Radium Institute 'V.G. Chlopin' Leningrad in the field of destructive burn-up determination. Laboratory methods of burn-up determination using the classical monitors 137Cs, 106Ru, 148Nd and isotopes of heavy metals (U, Pu) as well as the usefulness of 90Sr, stable isotopes of Ru and Mo as monitors are dealt with. The analysis of the fuel components uranium (spectrophotometry, potentiometric titration, mass-spectrometric isotope dilution) and plutonium (spectrophotometry, coulometric titration, mass- and alpha-spectrometric isotope dilution) is fully described. Possibilities of increasing the reproducibility (automatic adjusting of measurement conditions) and the sensibility (ion impuls counting) of mass-spectrometric measurements are proposed and applied to a precise determination of Am and Cm isotopic composition. The methods have been used for burn-up analysis of spent WWER (especially WWER-440) fuel. (author)

  14. Development of a combined chemical and enzymatic approach for the mass spectrometric identification and quantification of aberrant N-glycosylation.

    Science.gov (United States)

    Chen, Rui; Wang, Fangjun; Tan, Yexiong; Sun, Zhen; Song, Chunxia; Ye, Mingliang; Wang, Hongyang; Zou, Hanfa

    2012-02-16

    Direct mass spectrometric analysis of aberrant protein glycosylation is a challenge to the current analytical techniques. Except lectin affinity chromatography, no other glycosylation enrichment techniques are available for analysis of aberrant glycosylation. In this study, we developed a combined chemical and enzymatic strategy as an alternative for the mass spectrometric analysis of aberrant glycosylation. Sialylated glycopeptides were enriched with reverse glycoblotting, cleaved by endoglycosidase F3 and analyzed by mass spectrometry with both neutral loss triggered MS(3) in collision induced dissociation (CID) and electron transfer dissociation (ETD). Interestingly, a great part of resulted glycopeptides were found with fucose attached to the N-acetylglucosamine (N-GlcNAc), which indicated that the aberrant glycosylation that is carrying both terminal sialylation and core fucosylation was identified. Totally, 69 aberrant N-glycosylation sites were identified in sera samples from hepatocellular carcinoma (HCC) patients. Following the identification, quantification of the level of this aberrant glycosylation was also carried out using stable isotope dimethyl labeling and pooled sera sample from liver cirrhosis and HCC was compared. Six glycosylation sites demonstrated elevated level of aberrancy, which demonstrated that our developed strategy was effective in both qualitative and quantitative studies of aberrant glycosylation. PMID:22202184

  15. Dosimetric studies, spectrometric, radiographic, metallographic of a new argentinean seed of 125 I used in brachytherapy

    International Nuclear Information System (INIS)

    A new source of 125 I model BraquibacTM has been developed in Argentina for applications in interstitial brachytherapy. The AAPM Task Group 43 (TG-43) recommends that dosimetric characteristics of new sources of brachytherapy of Iodine-125 have been theoretically and experimentally determined before its clinical use. The objectives outlined in this work were the study of the design of the new seed, the calculation of dosimetric parameters and the photons spectra analysis. Its were carried out radiographic and metallographic studies to determine the physical characteristics of the source. For the realization of the dosimetric calculations it was used the Monte Carlo code MCNP5. Values of the radial dose function, g(r), of the constant of dose rate, Λ, of the function of anisotropy of two dimensions, F(r, θ), of the factor and constant of anisotropy its were obtained simulating the source in water according to the recommended methodology in TG-43. The constant of dose rate is similar to 0,880 ± 0,080 c Gy h-1 U-1. The kerma in air rate of reference, SK, was calculated as 1,036 c Gy cm2h-1 mCi-1 simulating the seed in dry air. Its were carried out spectrometric studies using a semiconductor planar detector of HPGe (high purity germanium). Photons spectra showed characteristic x-rays of 125 I with energies of 27,20 keV, 27,47 keV, 31 keV and 31,70 keV gamma photons of 35,5 keV, and x-ray fluorescent coming from the silver nucleus of 22,10 keV, 24,94 keV and 25,45 keV. The angular dependence of the intensity of photons around the seed and in air it was analyzed with the planar detector. This was carried out to study the anisotropy in the photons flow due to variation in the thickness of the titanium wall and of the welding, movements of the silver tube inside the source and deposition of the radioactive material on the silver tube. (Author)

  16. Method development of gas analysis with mass spectrometer

    International Nuclear Information System (INIS)

    Dissolved gas content in deep saline groundwater is an important factor, which has to be known and taken into account when planning the deep repository for the spent nuclear fuel. Posiva has investigated dissolved gases in deep groundwaters since the 1990's. In 2002 Posiva started a project that focused on developing the mass spectrometric method for measuring the dissolved gas content in deep saline groundwater. The main idea of the project was to analyse the dissolved gas content of both the gas phase and the water phase by a mass spectrometer. The development of the method started in 2003 (in the autumn). One of the aims was to create a parallel method for gas analysis with the gas chromatographic method. The starting point of this project was to test if gases could be analysed directly from water using a membrane inlet in the mass spectrometer. The main objective was to develop mass spectrometric methods for gas analysis with direct and membrane inlets. An analysis method for dissolved gases was developed for direct gas inlet mass spectrometry. The accuracy of the analysis method is tested with parallel real PAVE samples analysed in the laboratory of Insinoeoeritoimisto Paavo Ristola Oy. The results were good. The development of the membrane inlet mass spectrometric method still continues. Two different membrane materials (silicone and teflon) were tested. Some basic tests (linearity,repeatability and detection limits for different gases) will be done by this method. (orig.)

  17. Discrimination of Citrus reticulata Blanco and Citrus reticulata 'Chachi' by gas chromatograph-mass spectrometry based metabolomics approach.

    Science.gov (United States)

    Duan, Li; Guo, Long; Dou, Li-Li; Zhou, Chang-Lin; Xu, Feng-Guo; Zheng, Guo-Dong; Li, Ping; Liu, E-Hu

    2016-12-01

    Citri Reticulatae Pericarpium, mainly including the pericarp of Citrus reticulata Blanco and the pericarp of Citrus reticulata 'Chachi', has been consumed daily as food and dietary supplement for centuries. In this study, GC-MS based metabolomics was employed to compare comprehensively the volatile constituents in Citrus reticulata Blanco and Citrus reticulata 'Chachi'. Principal component analysis and orthogonal partial least squares discrimination analysis indicated that samples could be distinguished effectively from one another. Fifteen metabolites were finally identified for use as chemical markers in discrimination of Citri Reticulatae Pericarpium samples. The antimicrobial activity against Gram-negative and Gram-positive bacteria of the volatile oil from Citrus reticulata Blanco and Citrus reticulata 'Chachi' was investigated preliminarily. PMID:27374515

  18. Influence of particle size of wear metal on the spectrometric oil analysis programme (SOAP), demonstrated by the determination of iron by AAS

    International Nuclear Information System (INIS)

    The possibility that there might be a relation between particle size of wear metal and spectrometric determination, (e.g. of the iron content in used lubricating oils) has been examined. In this connection it had to be clarified from which particle size of the iron wear the Fe content determined by direct AAS (solution of the oil sample) is in agreement with the true value in the used oil. The determination of the absolute iron content was performed by a colorimetric method preceded by an incineration of the used oil. Contrary to other publications, in which work is based on spherical iron particles as a simulated wear, the test described here relates to true wear particles. To obtain the total iron wear from a gear oil it was filtered off from the used oil and afterwards separated into defined particle size ranges by a procedure specially developed for this purpose. The different groups of scaly particles, which were collected in this way, were then mixed homogeneously into fresh luboil samples according to their sizes. The determination of the iron content from these newly mixed luboil samples was carried out 1. by direct AAS, 2. by AAS after incineration of the oil samples and 3. by a colorimetric method (to obtain the absolute value of the iron content). The results showed a recovery of the iron of only 50% if the wear particles were bigger than about 2 μm. That means that the true value of the iron content in a used lubricating oil is found by direct AAS only if the particle size is <=1 μm. (orig.)

  19. Mass Spectrometric Investigation of Silicon Extremely Enriched in (28)Si: From (28)SiF4 (Gas Phase IRMS) to (28)Si Crystals (MC-ICP-MS).

    Science.gov (United States)

    Pramann, Axel; Rienitz, Olaf

    2016-06-01

    A new generation of silicon crystals even further enriched in (28)Si (x((28)Si) > 0.999 98 mol/mol), recently produced by companies and institutes in Russia within the framework of a project initiated by PTB, were investigated with respect to their isotopic composition and molar mass M(Si). A modified isotope dilution mass spectrometric (IDMS) method treating the silicon as the matrix containing a so-called virtual element (VE) existing of the isotopes (29)Si and (30)Si solely and high resolution multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) were applied in combination. This method succeeds also when examining the new materials holding merely trace amounts of (29)Si (x((29)Si) ≈ 5 × 10(-6) mol/mol) and (30)Si (x((30)Si) ≈ 7 × 10(-7) mol/mol) extremely difficult to detect with lowest uncertainty. However, there is a need for validating the enrichment in (28)Si already in the precursor material of the final crystals, silicon tetrafluoride (SiF4) gas prior to crystal production. For that purpose, the isotopic composition of selected SiF4 samples was determined using a multicollector magnetic sector field gas-phase isotope ratio mass spectrometer. Contaminations of SiF4 by natural silicon due to storing and during the isotope ratio mass spectrometry (IRMS) measurements were observed and quantified. The respective MC-ICP-MS measurements of the corresponding crystal samples show-in contrast-several advantages compared to gas phase IRMS. M(Si) of the new crystals were determined to some extent with uncertainties urel(M) orders of magnitude and thus further reduces the uncertainty of the Avogadro constant NA which is one of the preconditions for the redefinition of the SI unit kilogram. PMID:27173726

  20. Development and validation of analytical methods for monomeric and oligomeric migrants from nylon 12 packaging materials.

    NARCIS (Netherlands)

    Stoffers, N.H.; Brandl, F.; Linssen, J.P.H.; Franz, R.

    2003-01-01

    Analytical methods for the determination of laurolactam-the monomer of nylon 12-as well as the cyclic dimer and trimer were established. High performance liquid chromatography using ultraviolet (HPLC-UV) and mass spectrometric detection (HPLC-MS) were both found suitable to identify and quantify mon

  1. Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

    Science.gov (United States)

    Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

    1996-01-01

    A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

  2. A Nanoparticle-based Solid Phase Extraction Method for Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometric Analysis

    OpenAIRE

    Song, Yaru; Zhao, Shulin; Tchounwou, Paul; Liu, Yi-Ming

    2007-01-01

    A solid-phase extraction (SPE) procedure with the use of superparamagnetic Fe3O4 nanoparticles as extracting agent was developed for HPLC-ESI-MS/MS analysis. Four most heavily used triazine pesticides (herbicides) were taken as the test compounds. The NPs showed an excellent capability to retain the compounds tested, and a quantitative extraction was achieved within 10 min under the testing conditions, i.e. 100 μL NP solution was added to 400 mL sample in a beaker with stirring. After extract...

  3. Development of liquid chromatography mass spectrometric methods for quantification of metabolites from cellular level to clinical biomarkers

    OpenAIRE

    Tohmola, Niina

    2015-01-01

    Metabolites are low molecular weight compounds participating in different functions of cellular systems. Metabolites can be used as diagnostic biomarkers for numerous diseases. Liquid chromatography tandem mass spectrometry (LC-MS/MS) is a powerful tool in quantification of metabolites from various sample matrices. Good sensitivity and specificity are the main benefits of the technique. Mass spectrometry is commonly used in industry, drug research and clinical diagnostics. Extensive validatio...

  4. A liquid chromatography-mass spectrometric method for the detection of cyclic beta-amino fatty acid lipopeptides.

    Czech Academy of Sciences Publication Activity Database

    Urajová, P.; Hájek, Jan; Wahlsten, M.; Jokela, J.; Galica, T.; Fewer, D.P.; Kust, Andreja; Zapomělová; Kozlíková, Eliška; Delawská, K.; Sivonen, K.; Kopecký, J.; Hrouzek, P.

    2016-01-01

    Roč. 1438, MAR (2016), s. 76-83. ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA14-18067S; GA ČR(CZ) GA16-09381S Institutional support: RVO:60077344 Keywords : lipopeptides * bacteria * cyanobacteria * LC-HRMS * fatty acid * peptide Subject RIV: EF - Botanics Impact factor: 4.169, year: 2014

  5. Direct continuous multichannel gamma spectrometric measurements -one of the main methods for control and study of radioactive environmental pollution

    International Nuclear Information System (INIS)

    Six reasons are given for suggesting that radioactivity in the environment should be monitored continuously using multichannel gamma spectrometry. These are the probability of an accident at a nuclear power plant (estimated at one every 4 years for the number of power stations now in operation), the possibility of damage to a reactor from natural disaster, the increased use of nuclear powered ships, missiles etc, the radioactivity released during the course of normal operation of nuclear facilities, the increased use of radioisotope sources and as a basis for modelling radionuclide migration and redistribution over time. The use of stationary monitoring points as well as on vehicles, boats and aircraft is recommended. Some problems are discussed. The experience of continuous gamma monitoring following the Chernobyl accident is discussed and results given. (U.K.)

  6. 40 CFR Appendix C to Part 136 - Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Element Analysis of...

    Science.gov (United States)

    2010-07-01

    ... absorption spectrometry, or other approved methodology. 5.2.4Wavelength scanning of analyte line region. If..., Publication No. 77-206, August 1977. 14.8“OSHA Safety and Health Standards, General Industry,” (29 CFR part... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Inductively Coupled...

  7. Extraction Chromatographic Methods in the Sample Preparation Sequence for Thermal Ionization Mass Spectrometric Analysis of Plutonium Isotopes

    International Nuclear Information System (INIS)

    A sample preparation sequence for actinide isotopic analysis by TIMS is described that includes column-based extraction chromatography as the first separation step, followed by anion exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA-resin and DGA-resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple isotopic spikes through the separation sequence. Pu recoveries were 87% and 86% for TEVA- and DGA-resins separations respectively. The Pu recoveries from 400 μL anion-exchange column separations were 89% and 93% for trial sequences incorporating TEVA and DGA-resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency, for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73 ± 0.77% (2-sigma) for the DGA-resin trials and 2.67 ± 0.54% for the TEVA-resin trials, compared to 3.41% and 2.37% (average 2.89%) for two spikes in the experimental set. These compare with an average measurement efficiency of 2.78 ± 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS sample preparation.

  8. Shotgun Proteomics of Tomato Fruits: Evaluation, Optimization and Validation of Sample Preparation Methods and Mass Spectrometric Parameters.

    Science.gov (United States)

    Kilambi, Himabindu V; Manda, Kalyani; Sanivarapu, Hemalatha; Maurya, Vineet K; Sharma, Rameshwar; Sreelakshmi, Yellamaraju

    2016-01-01

    An optimized protocol was developed for shotgun proteomics of tomato fruit, which is a recalcitrant tissue due to a high percentage of sugars and secondary metabolites. A number of protein extraction and fractionation techniques were examined for optimal protein extraction from tomato fruits followed by peptide separation on nanoLCMS. Of all evaluated extraction agents, buffer saturated phenol was the most efficient. In-gel digestion [SDS-PAGE followed by separation on LCMS (GeLCMS)] of phenol-extracted sample yielded a maximal number of proteins. For in-solution digested samples, fractionation by strong anion exchange chromatography (SAX) also gave similar high proteome coverage. For shotgun proteomic profiling, optimization of mass spectrometry parameters such as automatic gain control targets (5E+05 for MS, 1E+04 for MS/MS); ion injection times (500 ms for MS, 100 ms for MS/MS); resolution of 30,000; signal threshold of 500; top N-value of 20 and fragmentation by collision-induced dissociation yielded the highest number of proteins. Validation of the above protocol in two tomato cultivars demonstrated its reproducibility, consistency, and robustness with a CV of < 10%. The protocol facilitated the detection of five-fold higher number of proteins compared to published reports in tomato fruits. The protocol outlined would be useful for high-throughput proteome analysis from tomato fruits and can be applied to other recalcitrant tissues. PMID:27446192

  9. Mass spectrometric protein characterization in proteome analysis using GELoader tip micro-columns packed with various chromatographic material

    International Nuclear Information System (INIS)

    In the early 90'ies mass spectrometry (MS) was introduced as a tool for identifying proteins in protein sequence databases. Since then it has become an integrated tool in protein characterization and is today routinely used to identify proteins separated by gel electrophoresis. A two-tiered mass spectrometric protein identification strategy has recently been proposed. In the first strategy peptide mass maps obtained from the protein of interest are compared with theoretically derived peptide mass maps from proteins in protein sequence databases. If the protein cannot be identified by this strategy, tandem mass spectrometric sequencing is used to generate enough sequence data to identify the protein in protein sequence databases or expressed sequence tag (EST) databases. However, the above strategies primarily identify a protein relatively to the DNA sequence, in which no information about e.g. post-translational modifications (PTMs) is stored. PTMs are known to modify the function, location, solubility and activity of proteins in the cell, and they are therefore very important for understanding living cells. More than 200 different PTMs are known, of which glycosylation, phosphorylation and proteolytic processing are the most common ones. Mass spectrometric analysis of PTMs on gel-separated proteins requires a higher amount of protein than for identification only. In addition, higher sequence coverage from the peptide mass maps or pre-purification of the modified peptides prior to MS analysis, is necessary for detection of putative modified peptides. In this study a multi-tiered strategy, in which GELoader tip micro-columns packed with increasingly more hydrophobic chromatographic material are used in combination with mass spectrometry, is described. The ultimate aim was to gain increased sequence coverage from peptide mixtures derived from gel-separated proteins, in order to locate modified peptides. Graphite powder is described as an alternative to traditional

  10. 2DB: a Proteomics database for storage, analysis, presentation, and retrieval of information from mass spectrometric experiments

    Directory of Open Access Journals (Sweden)

    Hippler Michael

    2008-07-01

    Full Text Available Abstract Background The amount of information stemming from proteomics experiments involving (multi dimensional separation techniques, mass spectrometric analysis, and computational analysis is ever-increasing. Data from such an experimental workflow needs to be captured, related and analyzed. Biological experiments within this scope produce heterogenic data ranging from pictures of one or two-dimensional protein maps and spectra recorded by tandem mass spectrometry to text-based identifications made by algorithms which analyze these spectra. Additionally, peptide and corresponding protein information needs to be displayed. Results In order to handle the large amount of data from computational processing of mass spectrometric experiments, automatic import scripts are available and the necessity for manual input to the database has been minimized. Information is in a generic format which abstracts from specific software tools typically used in such an experimental workflow. The software is therefore capable of storing and cross analysing results from many algorithms. A novel feature and a focus of this database is to facilitate protein identification by using peptides identified from mass spectrometry and link this information directly to respective protein maps. Additionally, our application employs spectral counting for quantitative presentation of the data. All information can be linked to hot spots on images to place the results into an experimental context. A summary of identified proteins, containing all relevant information per hot spot, is automatically generated, usually upon either a change in the underlying protein models or due to newly imported identifications. The supporting information for this report can be accessed in multiple ways using the user interface provided by the application. Conclusion We present a proteomics database which aims to greatly reduce evaluation time of results from mass spectrometric experiments and enhance

  11. Peptides from two sanguinovorous leeches analyzed by ultra-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometric detector

    Directory of Open Access Journals (Sweden)

    Ling Xiao

    2015-01-01

    Full Text Available Background: Hirudo nipponica Whitman and Poecilobdella manillensis Lesson fall into the family of Hirudinidae Whitman, both of them are sanguinovorous leeches and used a anticoagulant medicines in China. Their medicinal parts are the dried bodies. However, the peptides in the dried body of the two leeches have not been very clear up to now. Objective: To analyze the peptides from two sanguinovorous leeches, H. nipponica and P. manillensis. Materials and Methods: In this article it is reported that the peptides were obtained from anticoagulant active extracted parts of dried bodies of the two leeches and their molecular weights were analyzed by ultra-performance liquid chromatography with electrospray ionization quadrupole time-of-flight mass spectrometry mass spectrometric detector online. Results: Three peptide components were identified from H. nipponica with their molecular weight separately 14998, 15988, and 15956, six peptide components were identified from P. manillensis with molecular weight 9590, 13642, 14998, 17631, 15988, and 16567. Two of peptides from P. manillensis have the same molecular weight 14998 and 15988 as that in H. nipponica. Conclusion: And the two peptides are the main peaks in the base peak ion chromatogram because they occupied a large ratio of total base peak area. Hence the composition of the extracted active part of the two leeches are very close, difference is in that the extract of P. manillensis has more small peptide peaks, but the extract of H. nipponica has not. Furthermore, the tryptic digestion hydrolysates of the extracted active part of each sample were analyzed and the results showed that there were four peaks which only exist in P. manillensis, but not in Hirudo nipponia. They may be the identified peak between the two leeches. This work support the viewpoint that P. manillensis can be used as a medicinal leech as H. nipponia and these peptide components of dried bodies of the two species leeches are a

  12. Ampicillin/penicillin-binding protein interactions as a model drug-target system to optimize affinity pull-down and mass spectrometric strategies for target and pathway identification.

    Science.gov (United States)

    von Rechenberg, Moritz; Blake, Brian Kelly; Ho, Yew-Seng J; Zhen, Yuejun; Chepanoske, Cindy Lou; Richardson, Bonnie E; Xu, Nafei; Kery, Vladimir

    2005-05-01

    The identification and validation of the targets of active compounds identified in cell-based assays is an important step in preclinical drug development. New analytical approaches that combine drug affinity pull-down assays with mass spectrometry (MS) could lead to the identification of new targets and druggable pathways. In this work, we investigate a drug-target system consisting of ampicillin- and penicillin-binding proteins (PBPs) to evaluate and compare different amino-reactive resins for the immobilization of the affinity compound and mass spectrometric methods to identify proteins from drug affinity pull-down assays. First, ampicillin was immobilized onto various amino-reactive resins, which were compared in the ampicillin-PBP model with respect to their nonspecific binding of proteins from an Escherichia coli membrane extract. Dynal M-270 magnetic beads were chosen to further study the system as a model for capturing and identifying the targets of ampicillin, PBPs that were specifically and covalently bound to the immobilized ampicillin. The PBPs were identified, after in situ digestion of proteins bound to ampicillin directly on the beads, by using either one-dimensional (1-D) or two-dimensional (2-D) liquid chromatography (LC) separation techniques followed by tandem mass spectrometry (MS/MS) analysis. Alternatively, an elution with N-lauroylsarcosine (sarcosyl) from the ampicillin beads followed by in situ digestion and 2-D LC-MS/MS analysis identified proteins potentially interacting noncovalently with the PBPs or the ampicillin. The in situ approach required only little time, resources, and sample for the analysis. The combination of drug affinity pull-down assays with in situ digestion and 2-D LC-MS/MS analysis is a useful tool in obtaining complex information about a primary drug target as well as its protein interactors. PMID:15761956

  13. Application of a Liquid Extraction Based Sealing Surface Sampling Probe for Mass Spectrometric Analysis of Dried Blood Spots and Mouse Whole-Body Thin Tissue Sections

    Energy Technology Data Exchange (ETDEWEB)

    Van Berkel, Gary J [ORNL; Kertesz, Vilmos [ORNL

    2009-01-01

    The utility of a liquid extraction based sealing surface sampling probe (SSSP) for the direct mass spectrometric analysis of targeted drugs and metabolites in dried blood spots (DBSs) and whole mouse thin tissue sections was demonstrated. The accuracy and precision for the quantitative analysis of a minimum of 50 ng/mL sitamaquine or acetaminophen in DBSs on paper were well within the required 15% dictated by internationally recognized acceptance criteria for assay validations. Analysis of whole-body mouse thin tissue sections from animals dosed with propranolol, adhered to an adhesive tape substrate, provided semi-quantitative information for propranolol and its hydroxyproranolol glucuronide metabolite within specific organs of the tissue. The relative abundances recorded for the two compounds in the brain, lung, kidney and liver were in nominal agreement with previously reported amounts based on analysis using a liquid microjunction surface sampling probe (LMJ-SSP), and whole-body autoradiography (WBA) and HPLC-MS analysis. The ability to sample and analyze from tape-adhered tissue samples, which are generally employed in WBA analysis, presents the possibility of consecutive WBA and SSSP-MS analysis of the same tissue section. This would facilitate assignment, and possibly quantitation, of the different molecular forms of total drug related material detected in the WBA analysis. The flexibility to sample larger or smaller spot sizes, alternative probe sealing mechanisms, and a reduction in internal volumes and associated sample carryover issues will be among the first simple improvements necessary to make the SSSP-MS method a practical DBS and/or thin tissue section analysis tool or to expand its use to other surface sampling applications.

  14. Application of wall-stabilized plasma arc for the spectrometric determination of impurity elements in uranium yellow cake

    International Nuclear Information System (INIS)

    The application of a seeded wall-stabilized argon plasma arc as an excitation source for the emission spectrometric determination of some impurity elements in a sample of uranium yellow cake has been investigated. The sample was dissolved in nitric acid. Uranium was extracted from the sample solution using tributyl phosphate (TBP), and the aqueous solution was injected into the arc. The elements determined were Al, Ca, Fe, Mg, Mn, Mo, Sr and Zr. Limits of detection and precision of the technique are presented. The study of the influence of residual uranium in the nebulized solution on the intensity of spectral lines revealed that uranium concentrations up to 100 μg mL-1 have no significant interfering effect

  15. Evaluation of radioactive environmental hazards in Area-3, Northern Palmyrides, Central Syria using airborne spectrometric gamma technique.

    Science.gov (United States)

    Asfahani, J; Aissa, M; Al-Hent, R

    2016-01-01

    Airborne spectrometric gamma data are used in this paper to estimate the degree of radioactive hazard on humanity in Area-3, Northern Palmyrides, Central Syria. Exposure Rate (ER), Absorbed Dose Rate (ADR), Annual Effective Dose Rate (AEDR), and Heat Production (HP) of the eleven radiometric units included in the established lithological scored map in the study area have been computed to evaluate the radiation background influence in humans. The results obtained indicate that a human body in Area-3 is subjected to radiation hazards in the acceptable limits for long duration exposure. The highest radiogenetic heat production values in Area-3 correspond to the phosphatic locations characterized by relatively high values of uranium and thorium. PMID:26569554

  16. Statistical factor analysis of aerial spectrometric data, Al-Awabed area, Syria: a useful guide for phosphate and uranium exploration

    International Nuclear Information System (INIS)

    Factor analysis provides a quantitative interpretation for synthesizing and correlating data from airborne spectrometric surveys. Factor analysis is applied on such data of Al-Awabed area, Northern Palmyrides. The seven variables used in this research are: total radioactivity Ur, eU, eTh, K%, eU/eTh, eU/K and eTh/K. The analysis and interpretation show that a model of four factors (F1, F2, F3 and F4) is sufficient to represent them, where 94% of total data variance is interpreted. Mapping of these four factors proved to be a powerful tool for a direct differentiation of various rocks units, and a score lithological map of 11 radiometric units was established

  17. Desorption Electrospray Ionization (DESI Mass Spectrometric Imaging of the Distribution of Rohitukine in the Seedling of Dysoxylum binectariferum Hook. F.

    Directory of Open Access Journals (Sweden)

    Patel Mohana Kumara

    Full Text Available Ambient ionization mass spectrometric imaging of all parts of the seedling of Dysoxylum binectariferum Hook. f (Meliaceae was performed to reconstruct the molecular distribution of rohitukine (Rh and related compounds. The species accumulates Rh, a prominent chromone alkaloid, in its seeds, fruits, and stem bark. Rh possesses anti-inflammatory, anti-cancer, and immuno-modulatory properties. Desorption electrospray ionization mass spectrometry imaging (DESI MSI and electrospray ionization (ESI tandem mass spectrometry (MS/MS analysis detected Rh as well as its glycosylated, acetylated, oxidized, and methoxylated analogues. Rh was predominantly distributed in the main roots, collar region of the stem, and young leaves. In the stem and roots, Rh was primarily restricted to the cortex region. The identities of the metabolites were assigned based on both the fragmentation patterns and exact mass analyses. We discuss these results, with specific reference to the possible pathways of Rh biosynthesis and translocation during seedling development in D. binectariferum.

  18. Comparison of spectrometric characteristics of the FEhU-110, FEhU-139 and RCA-4524 photomultiplier

    International Nuclear Information System (INIS)

    The results of measuring energy resolution of the FEU-139 photomultipliers with the 63 mm diameter antimony-potassium-caesium photocathode, with the NaI(Tl) spectrometric detector for ν radiation energies of 60 keV (241Am), 122 keV (57Co) and 662 keV (137Cs) are presented. It is shown that energy resolution in the investigated energy range 1.2-1.5 times better for the FEU-139 than for FEU-110. Small spread of energy resolution for the FEU-139(20%) as compared with the FEU-110(50%) offers an advantages for their selection for detecting units. The FEU-139 has the same performances spectroscopic as the RCA-4524 photomultiplier

  19. Ultraviolet irradiation-induced substitution of fluorine with hydroxyl radical for mass spectrometric analysis of perfluorooctane sulfonyl fluoride.

    Science.gov (United States)

    Wang, Peng; Tang, Xuemei; Huang, Lulu; Kang, Jie; Zhong, Hongying

    2016-01-28

    A rapid and solvent free substitution reaction of a fluorine atom in perfluorooctane sulfonyl fluoride (PFOSF) with a hydroxyl radical is reported. Under irradiation of ultraviolet laser on semiconductor nanoparticles or metal surfaces, hydroxyl radicals can be generated through hole oxidization. Among all fluorine atoms of PFOSF, highly active hydroxyl radicals specifically substitute the fluorine of sulfonyl fluoride functional group. Resultant perfluorooctane sulfonic acid is further ionized through capture of photo-generated electrons that switch the neutral molecules to negatively charged odd electron hypervalent ions. The unpaired electron subsequently initiates α O-H bond cleavage and produces perfluorooctane sulfonate negative ions. Hydroxyl radical substitution and molecular dissociation of PFOSF have been confirmed by masses with high accuracy and resolution. It has been applied to direct mass spectrometric imaging of PFOSF adsorbed on surfaces of plant leaves. PMID:26755143

  20. Microemulsion electrokinetic chromatography with on-line atmospheric pressure photoionization-mass spectrometric detection of medium polarity compounds.

    Science.gov (United States)

    Himmelsbach, Markus; Haunschmidt, Manuela; Buchberger, Wolfgang; Klampfl, Christian W

    2007-08-01

    In this paper, we present the determination of pharmaceuticals employing microemulsion electrokinetic chromatography (MEEKC) with atmospheric pressure photoionization-mass spectrometric (APPI-MS) detection. This recent hyphenated technique allows to overcome some disadvantages of MEEKC, namely its inherent incompatibility with MS detection. Important parameters like microemulsion (ME) composition, the composition of the sheath liquid and APPI-MS detection parameters have been investigated. Using the optimized set of parameters, the eight selected substances could be detected down to concentrations between 3 mg L(-1) (phenacetin) and 41 mg L(-1) (diltiazem). Switching to the MS2 mode, the use of specific transitions for the detection of each analyte provided improved detection limits in the range of 0.6 mg L(-1) (carbamazepine) to 6 mg L(-1) (metoprolol). Calibration curves were linear over one to two orders of magnitude with correlation coefficients better than 0.98. PMID:17416381

  1. Determination of dithiocarbamates and milneb residues in foods by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Nakamura, Munetomo; Noda, Satoko; Kosugi, Masaki; Ishiduka, Noriko; Mizukoshi, Kazushi; Taniguchi, Makoto; Nemoto, Satoru

    2010-01-01

    A highly sensitive gas chromatographic-mass spectrometric (GC-MS) method was developed for dithiocarbamates (DTCs) and milneb in foods. DTCs and milneb were extracted from foods with cysteine-EDTA solution as sodium salts, and methylated with methyl iodide. Methyl derivatives of DTCs and milneb were cleaned up on a neutral alumina mini column and determined by GC-MS. The mean recoveries of DTCs and milneb were in the range of 72-120%, except for methiram. The quantification limits were 0.01 mg/kg (as CS(2)) in foods except tea (0.1 mg/kg as CS(2)). The developed method was applied to 10 compounds (4 dimethyldithiocarbamates, 3 ethylenebisdithiocarbamates, polycarbamates, propineb and milneb). PMID:21071904

  2. The mechanism of 2-furaldehyde formation from D-xylose dehydration in the gas phase. A tandem mass spectrometric study.

    Science.gov (United States)

    Ricci, Andreina; Piccolella, Simona; Pepi, Federico; Garzoli, Stefania; Giacomello, Pierluigi

    2013-07-01

    The mechanism of reactions occurring in solution can be investigated also in the gas phase by suited mass spectrometric techniques, which allow to highlight fundamental mechanistic features independent of the influence of the medium and to clarifying controversial hypotheses proposed in solution studies. In this work, we report a gas-phase study performed by electrospray triple stage quadrupole mass spectrometry (ESI-TSQ/MS) on the dehydration of D-xylose, leading mainly to the formation of 2-furaldehyde (2-FA). It is generally known in carbohydrate chemistry that the thermal acid catalyzed dehydration of pentoses leads to the formation of 2-FA, but several aspects on the solution-phase mechanism are controversial. Here, gaseous reactant ions corresponding to protonated xylose molecules obtained from ESI of a solution containing D-xylose and ammonium acetate as protonating reagent were allowed to undergo collisionally activated decomposition (CAD) into the triple stage quadrupole analyzer. The product ion mass spectra of protonated xylose are characterized by the presence of ionic intermediates arising from xylose dehydration, which were structurally characterized by their fragmentation patterns. As expected, the xylose triple dehydration leads to the formation of the ion at m/z 97, corresponding to protonated 2-FA. On the basis of mass spectrometric evidences, we demonstrated that in the gas phase, the formation of 2-FA involves protonation at the OH group bound to the C1 atom of the sugar, the first ionic intermediate being characterized by a cyclic structure. Finally, energy resolved product ion mass spectra allowed to obtain information on the energetic features of the D-xylose→2-FA conversion. ᅟ PMID:23690250

  3. NASVD and MNF techniques and your application noise reduction in gamma-ray spectrometric data; As tecnicas NASVD e MNF e sua aplicacao na reducao de ruidos em dados gamaespectrometricos

    Energy Technology Data Exchange (ETDEWEB)

    Cavallaro, Francisco de Assis, E-mail: assisfc@yahoo.com.br, E-mail: assis@agp-la.org [Departamento de Geologia Sedimentar e Ambiental, DGSA, Instituto de Geociencias, IG, Universidade de Sao Paulo, SP (Brazil); AGPLA, AeroGeoPhysica Latinoamerica, Sao Paulo, SP (Brazil); Portugal, Rodrigo S.; Bizuti, Ariathemis M., E-mail: portugal@ige.unicamp.br, E-mail: ambizuti@ige.unicamp.br [Departamento de Geologia e Recursos Naturais, DGRN, Instituto de Geociencias, IG, Universidade Estadual de Campinas, SP (Brazil); Silva, Adalene M., E-mail: adalene@unb.br [Universidade de Brasilia (UnB), DF (Brazil). Inst. de Geociencias. Dept. de Geoquimica e Recursos Minerais (GRM)

    2009-04-15

    The radioactive decay is a random process, and the measurement precision is ruled by statistical laws. The counting ratios of the profiles are always noisy when analyzed for short periods, such as one second per measurement. Corrections made at the end of conventional processing in the airborne gamma-ray spectrometric method data are not enough to remove and minimize, or even reduce considerably, the spectrum's originated noise. Two statistic methods that act locally in collected data, in the spectrum domain, have been suggested by literature to remove such remaining noises, the Noise-Adjusted Singular Value Decomposition - NASVD and Maximum Noise Fraction - MNF. These methods produce a significantly noise reduction. In this work both methods were applied in an area comprehended by two blocks, I and II, of the airborne survey that covers the west area of Mineral Province of Tapajos between Para and Amazon states. The filtered and non-filtered data with the NASVD and MNF techniques were processed with the Lasa's parameters. The comparison of results between maps and profiles shows that both methods are valuable, since there was resolution gain in these products. (author)

  4. FTIR SPECTROSCOPIC METHOD FOR QUANTITATIVE ANALYSIS OF CILNIDIPINE IN TABLET DOSAGE FORM

    OpenAIRE

    Ashish Patel; Arti Panchal; Viral Patel; Akhil Nagar

    2015-01-01

    A Fourier transform infrared (FT-IR) spectrometric method was developed for the rapid and direct measurement of Cilnidipine in pharmaceutical drugs. Cilnidipine is newly discovered and very effective antihypertensive drug. Cilnidipine can be determined by various methods and now we are adding a new one that uses a Fourier transform infrared spectrophotometric technique. The method involves the measurement of absorbance of carbonyl group (C=O) peak at 1697 cm-1. The proposed method was validat...

  5. A new robust method for the treatment of analytical data

    International Nuclear Information System (INIS)

    A new robust method is proposed for the calculation of the median and the relative standard deviation for a set of data containing unsymmetrically placed outliers. Examples of the advantages of the new method are given, the findings being confirmed by Monte Carlo tests. At Mintek mass-spectrometric data are often unsymmetrical, and all outliers are often at one of the extremities, either all high or all low. In some instances the outliers can be seen visually, and would therefore be rejected on sight. However, when large sets of results are processed, such as those from mass-spectrometric, X-ray fluorescence, and neutron-activation analyses, or in fields such as the assignment of values to reference materials, the sets of results are often too large for visual inspection and are processed within the computer

  6. Laser-induced spectrometric techniques to investigate the speciation of Eu in organic media

    International Nuclear Information System (INIS)

    Laser-induced spectrometric techniques provide both selectivity and sensitivity. The extremely low detection limits are ideal for assessing the extraction mechanisms involved in enhanced reprocessing applications through detailed speciation studies. Although time-resolved laser-induced fluorescence spectroscopy (TRLIF) is one of the most sensitive spectroscopy techniques, with the optical spectrum and its lifetime constituting two sources of data, it is limited to a few fluorescing actinides and lanthanides. This drawback warrants the development of an additional, complementary spectroscopic system with greater sensitivity than UV-Visible-near IR absorptiometry, based on measuring the pressure wave caused by the deexcitation of non-fluorescing species. Laser-induced photoacoustic spectroscopy (LIPAS) is based on measuring the characteristics of the pressure wave emitted during non-radiative relaxation of the absorbed energy. This speciation technique should allow investigation of compounds that absorb in the UV-visible range and are present at low concentrations in solution. It provides data on the nature and concentration of the species, including its oxidation, complexation and even colloidal states. The two techniques with a common laser source OPO were recently installed at Marcoule. TRLIF speciation studies are generally based on analyzing modifications in the fluorescence spectrum following a short laser pulse. They are related to the characteristic spectral pattern and relaxation rate of each species in solution. In the particular case of fluorescent decay of trivalent Am, Cm, Sm, Eu, Tb and Dy ions, the metallic cation deexcitation constant is closely related to the number of water molecules in the primary coordination sphere. This property helps to obtain more information on the structure around the metal ion. The first study was an investigation of the complexation of Eu(III) by TEMA (N, N'-tetra-ethyl-malonamide (C2H5)2NCO-CH2CON(C2H5)2) in the aqueous

  7. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Salka E.; Freese, R.; Cornett, C.;

    2000-01-01

    A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved by...... column-switching, using the first column (a Zorbax 300SB C-3 column) for sample cleanup and eluting the heart-cut flavonoid fraction onto the second column (a Zorbax SE C-18 column) for separation and detection by ultraviolet and atmospheric pressure chemical ionization MS using single ion monitoring in...... variation for the analysis of the 12 different flavonoids in quality control urine samples were 12.3% on average (range 11.0-13.7%, n = 24, reproducibility) and the repeatability of the assay were 5.0% (mean, range 0.1-14.8%, it = 12). A subset of 10 urine samples from a human dietary intervention study...

  8. A rapid method to authenticate vegetable oils through surface-enhanced Raman scattering

    Science.gov (United States)

    Lv, Ming Yang; Zhang, Xin; Ren, Hai Rui; Liu, Luo; Zhao, Yong Mei; Wang, Zheng; Wu, Zheng Long; Liu, Li Min; Xu, Hai Jun

    2016-03-01

    Vegetable oils are essential in our daily diet. Among various vegetable oils, the major difference lies in the composition of fatty acids, including unsaturated fatty acids (USFA) and saturated fatty acids (SFA). USFA include oleic acid (OA), linoleic acid (LA), and α-linolenic acid (ALA), while SFA are mainly palmitic acid (PA). In this study, the most typical and abundant USFA present with PA in vegetable oils were quantified. More importantly, certain proportional relationships between the integrated intensities of peaks centered at 1656 cm‑1 (S1656) in the surface-enhanced Raman scattering spectra of different USFA were confirmed. Therefore, the LA or ALA content could be converted into an equivalent virtual OA content enabling the characterization of the USFA content in vegetable oils using the equivalent total OA content. In combination with the S1656 of pure OA and using peanut, sesame, and soybean oils as examples, the ranges of S1656 corresponding to the National Standards of China were established to allow the rapid authentication of vegetable oils. Gas chromatograph-mass spectrometer analyses verified the accuracy of the method, with relative errors of less than 5%. Moreover, this method can be extended to other detection fields, such as diseases.

  9. Chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions

    International Nuclear Information System (INIS)

    These analytical procedures are designed to show whether a given material meets the purchaser's specifications as to plutonium content, effective fissile content, and impurity content. The following procedures are described in detail: plutonium by controlled-potential coulometry; plutonium by amperometric titration with iron(II); free acid by titration in an oxalate solution; free acid by iodate precipitation-potentiometric titration method; uranium by Arsenazo I spectrophotometric method; thorium by thorin spectrophotometric method; iron by 1,10-phenanthroline spectrophotometric method; chloride by thiocyanate spectrophotometric method; fluoride by distillation-spectrophotometric method; sulfate by barium sulfate turbidimetric method; isotopic composition by mass spectrometry; americium-241 by extraction and gamma counting; americium-241 by gamma counting; gamma-emitting fission products, uranium, and thorium by gamma-ray spectroscopy; rare earths by copper spark spectrochemical method; tungsten, niobium (columbium), and tantalum by spectrochemical method; simple preparation by spectrographic analysis for general impurities

  10. Comparison of accelerator mass spectrometric measurement with liquid scintillation counting measurement for the determination of {sup 14}C in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Yasuike, Kaeko, E-mail: k-yasuike@hokuriku-u.ac.j [Faculty of Pharmaceutical Sciences, Hokuriku University, Ho-3, Kanagawa-machi, Kanazawa, Ishikawa 920-1181 (Japan); Yamada, Yoshimune [Faculty of Pharmaceutical Sciences, Hokuriku University, Ho-3, Kanagawa-machi, Kanazawa, Ishikawa 920-1181 (Japan); Amano, Hikaru [AMS Management Section, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan)

    2010-04-15

    The concentrations of organically-bound {sup 14}C in tree-ring cellulose of a Japanese Black Pine grown in Shika-machi (37.0 deg. N, 136.8 deg. E) and those of a Japanese Cedar grown in Kanazawa (36.5 deg. N, 136.7 deg. E), Japan, were analyzed for the ring-years from 1989 to 1998 by the accelerator mass spectrometric measurement. The results were compared with those of the same samples analyzed by the liquid scintillation counting measurement to determine the reliability of liquid scintillation counting measurement. An important result of this study is that the sensitivity and reproducibility of accelerator mass spectrometric measurement was almost equal to that of liquid scintillation counting measurement.

  11. A Novel Type of Tri-Colour Light-Emitting-Diode-Based Spectrometric Detector for Low-Budget Flow-Injection Analysis

    Directory of Open Access Journals (Sweden)

    Nataša Gros

    2007-02-01

    Full Text Available In this paper we describe a low-cost spectrometric detector that can be easily assembled in a laboratory for less than €80 with a minimal number of optical components and which has proved sensitive and flexible enough for real-life applications. The starting point for the idea to construct this small, compact low-cost spectrometric detector was the decision to use a tri-colour light-emitting diode (LED of the red-green-blue (RGB type as a light source with the objective of achieving some flexibility in the selection of the wavelength (430 nm, 565 nm, 625 nm but avoiding the use of optical fibres. Due to the dislocation of the emitters of the different coloured light, the tri-colour LED-based detector required an optical geometry that differs from those that are described in literature. The proposed novel geometry, with a coil-type glass flow-through cell with up to four ascending turns, proved useful and fit for the purpose. The simplicity of the device means it requires a minimal number of optical components, i.e., only a tri-colour LED and a photoresistor. In order to make a flow-injection analysis (FIA with the spectrometric detector even more accessible for those with a limited budget, we additionally describe a low-cost simplified syringe-pump- based FIA set-up (€625, the assembling of which requires no more than basic technical facilities. We used such a set-up to test the performance of the proposed spectrometric detector for flow-injection analyses. The tests proved its suitability for real-life applications. The design procedures are also described.

  12. Mass Spectrometric Fragmentation of 1-(Benzyloxycarbonyl)amino-2-alkyl/cycloalkyl Thioacetates: a Thioester Pyrolysis-type Rearrangement under Electron Impact Ionization

    Institute of Scientific and Technical Information of China (English)

    Shu XU; Jia Xi XU

    2006-01-01

    The mass spectrometric fragmentation of 1-(benzyloxycarbonyl)amino-2-alkyl/cycloalkyl thioacetates has been studied with the aid of mass-analysed ion kinetic energy spectrometry under electron impact ionization. All compounds show a tendency to eliminate a ketene, thioacetic acid, and benzyl carbamate molecule, or an acetyl and benzyloxy radicals. A thioester pyrolysis-type rearrangement under electron impact ionizations was observed.

  13. Chemical, mass spectrometric, spectrochemical, nuclear and radiochemical analysis of nuclear-grade plutonium metal

    International Nuclear Information System (INIS)

    These analytical procedures are designed to show whether a given material meets the purchaser's specifications as to plutonium content, effective fissile content, and impurity content. The following procedures are described in detail: dissolution procedure; plutonium by controlled-potential coulometry; plutonium by amperometric titration with iron(II); plutonium by ceric sulfate titration method; uranium by Arsenazo I spectrophotometric method; thorium by thorin spectrophotometric method; iron by 1,10-phenanthroline spectrophotometric method; iron by 2,2'-bipyridyl spectrophotometric method; chloride by the thiocyanate spectrophotometric method; fluoride by distillation-spectrophotometric method; nitrogen by distillation-Nessler reagent spectrophotometric method; carbon by the direct combustion-thermal conductivity method; sulfur by distillation-spectrophotometric method; isotopic composition by mass spectrometry; Americium-241 by extraction and gamma counting; Americium-241 by gamma counting; gamma-emitting fission products, uranium, and thorium by gamma-ray spectroscopy; rare earths by copper spark spectrochemical method; tungsten, niobium (columbium) and tantalum by spectrochemical method; sample preparation for spectrographic analysis for trace impurities

  14. Synthesis, purification and mass spectrometric characterisation of a fluorescent Au9@BSA nanocluster and its enzymatic digestion by trypsin

    Science.gov (United States)

    Fernández-Iglesias, Nerea; Bettmer, Jörg

    2013-12-01

    Nanoclusters of noble metals like Ag and Au have attracted great attention as they form a missing link between isolated metal atoms and nanoparticles. Their particular properties like luminescence in the visible range and nontoxicity make them attractive for bioimaging and biolabelling purposes, especially with use of proteins as stabilising agents. In this context, this study intends the synthesis of a specific Au nanocluster covered by bovine serum albumin (BSA). It is shown that size-exclusion chromatography is feasible for the purification and isolation of the nanocluster. A mass spectrometric characterisation, preferably by ESI-MS, indicates the presence of an Au9@BSA nanocluster. Enzymatic digestion of the nanocluster with trypsin results in a significant increase of the fluorescence intensity at 650 and 710 nm, whereas complementary MALDI-MS studies are presented for the identification of generated peptides and show a distinctive pattern in comparison to the pure protein. It can be concluded that Au9@BSA might be, in future, an interesting candidate for in vitro studies of protease activities.Nanoclusters of noble metals like Ag and Au have attracted great attention as they form a missing link between isolated metal atoms and nanoparticles. Their particular properties like luminescence in the visible range and nontoxicity make them attractive for bioimaging and biolabelling purposes, especially with use of proteins as stabilising agents. In this context, this study intends the synthesis of a specific Au nanocluster covered by bovine serum albumin (BSA). It is shown that size-exclusion chromatography is feasible for the purification and isolation of the nanocluster. A mass spectrometric characterisation, preferably by ESI-MS, indicates the presence of an Au9@BSA nanocluster. Enzymatic digestion of the nanocluster with trypsin results in a significant increase of the fluorescence intensity at 650 and 710 nm, whereas complementary MALDI-MS studies are presented

  15. Mass spectrometric base composition profiling: Implications for forensic mtDNA databasing

    OpenAIRE

    Eduardoff, Mayra; Huber, Gabriela; Bayer, Birgit; Schmid, Dagmar; Anslinger, Katja; Göbel, Tanja; Zimmermann, Bettina; Schneider, Peter M; Röck, Alexander W; Parson, Walther

    2013-01-01

    In forensic genetics mitochondrial DNA (mtDNA) is usually analyzed by direct Sanger-type sequencing (STS). This method is known to be laborious and sometimes prone to human error. Alternative methods have been proposed that lead to faster results. Among these are methods that involve mass-spectrometry resulting in base composition profiles that are, by definition, less informative than the full nucleotide sequence. Here, we applied a highly automated electrospray ionization mass spectrometry ...

  16. Enrichment of trace amounts of copper(II) ions in water samples using octadecyl silica disks modified by a Schiff base ionophore prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Fathi, S.A.M. [Department of Chemistry, Faculty of Science, Zanjan University, PO Box 45195-313 Zanjan (Iran, Islamic Republic of); Yaftian, M.R. [Department of Chemistry, Faculty of Science, Zanjan University, PO Box 45195-313 Zanjan (Iran, Islamic Republic of)], E-mail: yaftian@znu.ac.ir

    2009-05-15

    Bis(5-bromo-2-hydroxybenzaldehyde)-1,2-propanediimine is synthesized by the reaction of 5-bromo-2-hydroxybenzaldehyde and 1,2-diaminopropane in ethanol. This ligand is used as a modifier of octadecyl silica disks for preconcentration of trace amounts of copper(II) ions, followed by nitric acid elution and flame atomic absorption spectrometric (FAAS) determination. The effect of parameters influencing the extraction efficiency, i.e. pH of the sample solutions, amount of the Schiff base, type and volume of stripping reagent, sample and eluent flow rates were evaluated. Under optimum experimental conditions, the capacity of the membrane disks modified by 4 mg of the ligand was found to be 247.7 ({+-}2.1) {mu}g of copper. The detection limit and the concentration factor of the presented method are 2.4 ng/l and greater than 400, respectively. The method was applied to the extraction, recovery and detection of copper in different synthetic and water samples.

  17. Comparison of extraction techniques and mass spectrometric ionization modes in the analysis of wine volatile carbonyls

    Energy Technology Data Exchange (ETDEWEB)

    Zapata, Julian; Mateo-Vivaracho, Laura; Cacho, Juan [Laboratory for Flavor Analysis and Enology, Institute of Engineering of Aragon, I3A, Department of Analytical Chemistry, Faculty of Sciences, University of Zaragoza, 50009 Zaragoza (Spain); Ferreira, Vicente, E-mail: vferre@unizar.es [Laboratory for Flavor Analysis and Enology, Institute of Engineering of Aragon, I3A, Department of Analytical Chemistry, Faculty of Sciences, University of Zaragoza, 50009 Zaragoza (Spain)

    2010-02-15

    This work presents a comparative study of the analytical characteristics of two methods for the analysis of carbonyl compounds in wine, both based on the derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). In the first method derivatives are formed in the solid phase extraction (SPE) cartridge in which the analytes have been previously isolated, while in the second method derivatives are formed in a solid phase microextraction (SPME) fibre saturated with vapors of the reagent and exposed to the sample headspace. In both cases detection has been carried out by electron impact (EI) or negative chemical ionization (NCI) mass spectrometry. The possibility of determining haloanisols simultaneously has been also considered. The method based on SPE presents, in general, better analytical properties than the SPME one. Although linearity was satisfactory for both methods (R{sup 2} > 0.99), repeatability of the SPE method (RSD < 10%) was better than that obtained with SPME (9% < RSD < 20%). Detection limits obtained with EI are better for the SPE method except for trihaloanisols, while with NCI detection limits for both strategies are comparable, although the SPME strategy presents worse results for ketones and methional. Detection limits are always lower with NCI, being the improvement most notable for SPME. Recovery experiments show that in the case of SPE, uncertainties are lower than 12% in all cases, while with the SPME method the imprecision plus the existence of matrix effects make the global uncertainty to be higher than 15%.

  18. Challenging design and development of Ma_Miss, a miniaturised spectrometric instrument for Mars sub-soil analysis

    Science.gov (United States)

    Battistelli, E.; Coradini, A.; Mugnuolo, R.; Capanni, A.; Paolinetti, R.; Re, E.; Magnani, P.

    2011-05-01

    This paper describes Ma_Miss (Mars Multispectral Imager for Subsurface Studies), the miniaturized instrument for spectrometric and stratigraphic analysis of sub-soil developed by SELEX Galileo in the context of ESA ExoMars mission. The Ma_Miss experiment is coordinated by the Principal Investigator Angioletta Coradini (IFSI-INAF, Rome) and is funded by the Italian Space Agency (ASI). The exploration of Mars requires a detailed in-situ investigation of the Martian surface and sub-surface. Determining the composition of the Martian subsoil will provide a direct indication of the steps through which the sample material evolved along geological timescales. Ma_Miss is an instrument fully integrated in the Drill system (developed by SELEX Galileo) hosted by a Rover operating on Mars surface; Ma_Miss illuminates the wall of the drill borehole and acquires its reflectance signal in the Visible and Infrared (0.4-2.2 micron) range, analyzes it through a miniaturized spectrometer (20nm spectral resolution), and transmits the digital data to the Rover. The innovative instrument concept was driven by several key needs, related to challenging scientific requirements and extreme environmental constraints. Implementation of the concept has required a deep interdisciplinary concurrent development in order to solve critical aspects of engineering and manufacturing, covering miniaturized monolithic optics and novel concept for fiberoptic connectors capable to automatically mate/de-mate during the robotic assembly of the Drill elements on Mars.

  19. Highly selective enrichment of phosphopeptides with high-index facets exposed octahedral tin dioxide nanoparticles for mass spectrometric analysis.

    Science.gov (United States)

    Ma, Rongna; Hu, Junjie; Cai, Zongwei; Ju, Huangxian

    2014-02-01

    High-index facets exposed octahedral tin dioxide (SnO2) nanoparticles were successfully synthesized and applied to selectively enrich phosphopeptides for mass spectrometric analysis. The high selectivity and capacity of the octahedral SnO2 nanoparticles were demonstrated by effectively enriching phosphopeptides from digests of phosphoprotein (α- or β-casein), protein mixtures of β-casein and bovine serum albumin, milk, and human serum samples. The unique octahedral SnO2 with abundant unsaturated coordination Sn atoms exhibited enhanced affinity and selective coordination ability with phosphopeptides due to their high chemical activity. The strong affinity led to highly selective capture and enrichment of phosphopeptides for sensitive detection through the bidentate bonds formed between surface atoms and phosphate. The phosphopeptides could be detected in β-casein down to 4 × 10(-9)M or in the mixture of β-casein and BSA with a molar ratio of even 1:100. The performance in selective enrichment of phosphopeptides from drinking milk and human serum showed powerful evidence of high selectivity and efficiency in identifying the low-abundant phosphopeptides from complicated biological samples. This work provided a way to improve the physical and chemical properties of materials by tailoring their exposed facets for selective enrichment of phosphopeptides. PMID:24401440

  20. Mass Spectrometric-Based Selected Reaction Monitoring of Protein Phosphorylation during Symbiotic Signaling in the Model Legume, Medicago truncatula.

    Science.gov (United States)

    Van Ness, Lori K; Jayaraman, Dhileepkumar; Maeda, Junko; Barrett-Wilt, Gregory A; Sussman, Michael R; Ané, Jean-Michel

    2016-01-01

    Unlike the major cereal crops corn, rice, and wheat, leguminous plants such as soybean and alfalfa can meet their nitrogen requirement via endosymbiotic associations with soil bacteria. The establishment of this symbiosis is a complex process playing out over several weeks and is facilitated by the exchange of chemical signals between these partners from different kingdoms. Several plant components that are involved in this signaling pathway have been identified, but there is still a great deal of uncertainty regarding the early events in symbiotic signaling, i.e., within the first minutes and hours after the rhizobial signals (Nod factors) are perceived at the plant plasma membrane. The presence of several protein kinases in this pathway suggests a mechanism of signal transduction via posttranslational modification of proteins in which phosphate is added to the hydroxyl groups of serine, threonine and tyrosine amino acid side chains. To monitor the phosphorylation dynamics and complement our previous untargeted 'discovery' approach, we report here the results of experiments using a targeted mass spectrometric technique, Selected Reaction Monitoring (SRM) that enables the quantification of phosphorylation targets with great sensitivity and precision. Using this approach, we confirm a rapid change in the level of phosphorylation in 4 phosphosites of at least 4 plant phosphoproteins that have not been previously characterized. This detailed analysis reveals aspects of the symbiotic signaling mechanism in legumes that, in the long term, will inform efforts to engineer this nitrogen-fixing symbiosis in important non-legume crops such as rice, wheat and corn. PMID:27203723

  1. Product Identification and Mass Spectrometric Analysis of n-Butane and i-Butane Pyrolysis at Low Pressure

    Institute of Scientific and Technical Information of China (English)

    Yi-jun Zhang; Wen-hao Yuan; Jiang-huai Cai; Li-dong Zhang; Fei Qi; Yu-yang Li

    2013-01-01

    The pyrolysis of n-butane andi-butane at low pressure was investigated from 823-1823 K in an electrically heated flow reactor using synchrotron vacuum ultraviolet photoionization mass spectrometry.More than 20 species,especially several radicals and isomers,were detected and identified from the measurements of photoionization efficiency (PIE) spectra.Based on the mass spectrometric analysis,the characteristics of n-butane and i-butane pyrolysis were discussed,which provided experimental evidences for the discussion of decomposition pathways of butane isomers.It is concluded that the isomeric structures of n-butane and i-butane have strong influence on their main decomposition pathways,and lead to dramatic differences in their mass spectra and PIE spectra such as the different dominant products and isomeric structures of butene products.Furthermore,compared with n-butane,i-butane can produce strong signals of benzene at low temperature in its pyrolysis due to the enhanced formation of benzene precursors like propargyl and C4 species,which provides experimental clues to explain the higher sooting tendencies of iso-alkanes than n-alkanes.

  2. Investigation of signaling molecules and metabolites found in crustacean hemolymph via in vivo microdialysis using a multifaceted mass spectrometric platform.

    Science.gov (United States)

    Jiang, Shan; Liang, Zhidan; Hao, Ling; Li, Lingjun

    2016-04-01

    Neurotransmitters (NTs) are endogenous signaling molecules that play an important role in regulating various physiological processes in animals. Detection of these chemical messengers is often challenging due to their low concentration levels and fast degradation rate in vitro. In order to address these challenges, herein we employed in vivo microdialysis (MD) sampling to study NTs in the crustacean model Cancer borealis. Multifaceted separation tools, such as CE and ion mobility mass spectrometry (MS) were utilized in this work. Small molecules were separated by different mechanisms and detected by MALDI mass spectrometric imaging (MALDI-MSI). Performance of this separation-based MSI platform was also compared to LC-ESI-MS. By utilizing both MALDI and ESI-MS, a total of 208 small molecule NTs and metabolites were identified, of which 39 were identified as signaling molecules secreted in vivo. In addition, the inherent property of sub microscale sample consumption using CE enables shorter time of MD sample collection. Temporal resolution of MD was improved by approximately tenfold compared to LC-ESI-MS, indicating the significant advantage of applying separation-assisted MALDI-MS imaging platform. PMID:26691021

  3. Mass Spectrometric-Based Selected Reaction Monitoring of Protein Phosphorylation during Symbiotic Signaling in the Model Legume, Medicago truncatula.

    Directory of Open Access Journals (Sweden)

    Lori K Van Ness

    Full Text Available Unlike the major cereal crops corn, rice, and wheat, leguminous plants such as soybean and alfalfa can meet their nitrogen requirement via endosymbiotic associations with soil bacteria. The establishment of this symbiosis is a complex process playing out over several weeks and is facilitated by the exchange of chemical signals between these partners from different kingdoms. Several plant components that are involved in this signaling pathway have been identified, but there is still a great deal of uncertainty regarding the early events in symbiotic signaling, i.e., within the first minutes and hours after the rhizobial signals (Nod factors are perceived at the plant plasma membrane. The presence of several protein kinases in this pathway suggests a mechanism of signal transduction via posttranslational modification of proteins in which phosphate is added to the hydroxyl groups of serine, threonine and tyrosine amino acid side chains. To monitor the phosphorylation dynamics and complement our previous untargeted 'discovery' approach, we report here the results of experiments using a targeted mass spectrometric technique, Selected Reaction Monitoring (SRM that enables the quantification of phosphorylation targets with great sensitivity and precision. Using this approach, we confirm a rapid change in the level of phosphorylation in 4 phosphosites of at least 4 plant phosphoproteins that have not been previously characterized. This detailed analysis reveals aspects of the symbiotic signaling mechanism in legumes that, in the long term, will inform efforts to engineer this nitrogen-fixing symbiosis in important non-legume crops such as rice, wheat and corn.

  4. Aeromagnetic and gamma-ray spectrometric data interpretation for uranium exploration - south eastern margin of the Chattisgarh Basin, India

    International Nuclear Information System (INIS)

    Airborne surveys were conducted along the south-eastern margin of the Chattisgarh Basin - Singhora Basin and Sonakhan greenstone belt by the Atomic Minerals Directorate for Exploration and Research in 2000 with E-W flight lines covering 19800 linekm. Preliminary processed aeromagnetic data were corrected for IGRF, heading and lag and levelled using tie line data. Based on the amplitude, frequency and textural characteristics of enhanced magnetic images, litho-structural information of the area was deciphered. Semi-quantitative interpretation of aeromagnetic data employing Euler's technique facilitated identification of source body locations along with depth estimates. Airborne Gamma Ray Spectrometric (AGRS) data were processed for altitude attenuation, radon interference and stripping corrections. The radiometric ternary image of the processed data shows good correlation with surface geology of the area. Radiometric anomalies were extracted from the derived concentrations based on mean and standard deviation of Uranium, U/Tb and U2/Th data sets. Finally, integrated Geographical Information System (G15) analysis of inferred faults and lineaments from aeromagnetic data and uranium anomalies mapped from AGRS data were used for extracting zones favourable for uranium mineralisation. Qualitative and quantitative analysis of aeromagnetic and AGRS data and integration of the results on a GIS platform thus helped in identifying target areas for further exploration. (author)

  5. Processing and Assessment of Spectrometric, Stereoscopic Imagery Collected Using a Lightweight UAV Spectral Camera for Precision Agriculture

    Directory of Open Access Journals (Sweden)

    Jussi Mäkynen

    2013-10-01

    Full Text Available Imaging using lightweight, unmanned airborne vehicles (UAVs is one of the most rapidly developing fields in remote sensing technology. The new, tunable, Fabry-Perot interferometer-based (FPI spectral camera, which weighs less than 700 g, makes it possible to collect spectrometric image blocks with stereoscopic overlaps using light-weight UAV platforms. This new technology is highly relevant, because it opens up new possibilities for measuring and monitoring the environment, which is becoming increasingly important for many environmental challenges. Our objectives were to investigate the processing and use of this new type of image data in precision agriculture. We developed the entire processing chain from raw images up to georeferenced reflectance images, digital surface models and biomass estimates. The processing integrates photogrammetric and quantitative remote sensing approaches. We carried out an empirical assessment using FPI spectral imagery collected at an agricultural wheat test site in the summer of 2012. Poor weather conditions during the campaign complicated the data processing, but this is one of the challenges that are faced in operational applications. The results indicated that the camera performed consistently and that the data processing was consistent, as well. During the agricultural experiments, promising results were obtained for biomass estimation when the spectral data was used and when an appropriate radiometric correction was applied to the data. Our results showed that the new FPI technology has a great potential in precision agriculture and indicated many possible future research topics.

  6. Chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solutions

    International Nuclear Information System (INIS)

    The standard covers analytical procedures to determine compliance of nuclear-grade uranyl nitrate solution to specifications. The following methods are described in detail: uranium by ferrous sulfate reduction-potassium dichromate titrimetry and by ignition gravimetry; specific gravity by pycnometry; free acid by oxalate complexation; thorium by the Arsenazo(III) (photometric) method; chromium by the diphenylcarbazide (photometric) method; molybdenum by the thiocyanate (photometric) method; halogens separation by steam distillation; fluorine by specific ion electrode; halogen distillate analysis: chloride, bromide and iodide by amperometric microtitrimetry; bromine by the fluorescein (photometric) method; sulfate sulfur by (photometric) turbidimetry; phosphorus by the molybdenum blue (photometric) method; silicon by the molybdenum blue (photometric) method; carbon by persulfate oxidation-acid titrimetry; nonvolatile impurities by spectrography; volatile impurities by rotating-disk spark spectrography; boron by emission spectrography; impurity elements by spark source mass spectrography; isotopic composition by multiple filament surface-ionization mass spectrometry; uranium-232 by alpha spectrometry; total alpha activity by direct alpha counting; fission product activity by beta and gamma counting; entrained organic matter by infrared spectrophotometry

  7. Gamma-spectrometric surveys in differentiated granites. II: the Joaquim Murtinho Granite in the Cunhaporanga Granitic Complex, Parana, SE Brazil; Levantamentos gamaespectrometricos em granitos diferenciados. II: O exemplo do Granito Joaquim Murtinho, Complexo Granitico Cunhaporanga, Parana

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Francisco Jose Fonseca [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Geologia. Lab. de Pesquisas em Geofisica Aplicada; Fruchting, Allan [Votorantim Metais, Sao Paulo, SP (Brazil)], e-mail: allan.fruchting@vmetais.com.br; Guimaraes, Gilson Burigo [Universidade Estadual de Ponta Grossa (UEPG), PR (Brazil). Dept. de Geociencias], e-mail: gburigo@ig.com.br; Alves, Luizemara Soares [PETROBRAS S.A., Rio de Janeiro, RJ (Brazil)], e-mail: luizemara@petrobras.com.br; Martin, Victor Miguel Oliveira; Ulbrich, Horstpeter Herberto Gustavo Jose [Universidade de Sao Paulo (USP), SP (Brazil). Inst. de Geociencias. Dept. de Mineralogia e Geotectonica], e-mail: vicmartin6@ig.com.br, e-mail: hulbrich@usp.br

    2009-07-01

    Detailed mapping at the NW corner of the large Neo proterozoic Cunhaporanga Granitic Complex (CGC), Parana state, SE Brazil, redefined the Joaquim Murtinho Granite (JMG), a late intrusion in CGC with an exposed area of about 10 km{sup 2}, made up mainly by evolved 'alaskites' (alkali-feldspar leuco granites). This unit is in tectonic contact with the Neoproterozoic-Eocambrian volcano-sedimentary Castro Group, to the W, and is intrusive into other less evolved granitic units of the CGC to the E. Petrographically, JMG shows mainly mesoperthite and quartz, with subordinate amounts of altered micas and some accessory phases, mainly zircon. The equi to inequigranular granites are usually deformed with cataclastic textures, are often brecciated, and may have miarolitic structures. Formation of late albite, sericite, carbonate and hematite was caused by deuteric and hydrothermal alteration. A gamma-ray spectrometric survey at 231 stations which measured total counts (TC), Ueq K%, eU ppm and eTh ppm was used to construct several direct and derived maps. Compared to neighboring units the JMG has significant anomalies, especially in the TC, %K, eTh and eU maps, although the differences are less obvious in some derived maps. These evolved granites are enriched in these three elements. Geochemical behavior of K, Th and U is used to analyse the results observed in maps. Enhanced weathering under a subtropical climate with moderate to high average temperatures and heavy rainfall affects mainly feldspars and biotite, and may also destabilize most U and Th-bearing accessory phases. Th is most likely retained in restite minerals in soils, being relatively immobile, while part of U may migrate as uranyl ion in oxidizing media. K is especially affected by feldspar alteration to K-free clays (mainly kaolinite), and may be completely leached. Gamma-ray spectrometric methods are valid tools to study facies in granitic rocks, especially in those that are enriched in K, Th and U

  8. Atomic absorbtion spectrometric determination of platinum, palladium and rhodium in catalysts for automotive exhaust

    International Nuclear Information System (INIS)

    Analytical parameters of the electrothermal atomic absorption spectrometry method have been optimized for determination of platinum, palladium and rhodium in ceramic-supported catalysts for automobile exhaust gas treatment. Two chemical sample preparation methods have been proposed. In order to simplify the sample preparation procedure and to prevent the possible losses of platinum group metals the treatment of the previously ground sample with a mixture of mineral acids is recommended. (authors)

  9. Mass spectrometric study of the phase boundaries of the CdS-CdTe system

    Energy Technology Data Exchange (ETDEWEB)

    Nunoue, S.Y.; Hemmi, T.; Kato, E. (Dept. of Materials Science and Engineering, Waseda Univ., Shinjuku-ku Tokyo 160 (JP))

    1990-04-01

    An isothermal evaporation method by means of a Knudsen cell-mass spectrometer combination has been applied to the determination of the phase boundaries in the CdS-CdTe system in the temperature range of 650{degrees}--720{degrees}C. The phase boundaries obtained were compared with published phase boundaries. The advantages of the present method over the x-ray diffraction technique are discussed.

  10. New Method for the Analysis of Flukicide and Other Anthelmintic Residues in Bovine Milk and Liver using LC-MS/MS

    Science.gov (United States)

    A liquid chromatographic-tandem mass spectrometric (LC-MS/MS) multi-residue method for the simultaneous quantification and identification of 38 residues of the most widely used anthelmintic veterinary drugs (including benzimidazoles, macrocyclic lactones, and flukicides) in milk and liver has been d...

  11. Modeling of detection efficiency of HPGe semiconductor detector by Monte Carlo method

    International Nuclear Information System (INIS)

    Over the past ten years following the gradual adoption of new legislative standards for protection against ionizing radiation was significant penetration of gamma-spectrometry between standard radioanalytical methods. In terms of nuclear power plant gamma-spectrometry has shown as the most effective method of determining of the activity of individual radionuclides. Spectrometric laboratories were gradually equipped with the most modern technical equipment. Nevertheless, due to the use of costly and time intensive experimental calibration methods, the possibilities of gamma-spectrometry were partially limited. Mainly in late 90-ies during substantial renovation and modernization works. For this reason, in spectrometric laboratory in Nuclear Power Plants Bohunice in cooperation with the Department of Nuclear Physics FMPI in Bratislava were developed and tested several calibration procedures based on computer simulations using GEANT program. In presented thesis the calibration method for measuring of bulk samples based on auto-absorption factors is described. The accuracy of the proposed method is at least comparable with other used methods, but it surpasses them significantly in terms of efficiency and financial time and simplicity. The described method has been used successfully almost for two years in laboratory spectrometric Radiation Protection Division in Bohunice nuclear power. It is shown by the results of international comparison measurements and repeated validation measurements performed by Slovak Institute of Metrology in Bratislava.

  12. DEFINING ELEMENTAL COMPOSITION OF VEGETABLE HYDROCOLLOIDS USING THE ELECTRON PROBE MICROANALYSIS METHOD

    OpenAIRE

    Дышлюк, Любовь; Бабич, Ольга; Белова, Дарья

    2014-01-01

    In production of soft capsules, natural and semi-synthetic vegetative analogues for pharmaceutical gelatin are used. This work is devoted to defining elemental composition of vegetative analogs for pharmaceutical gelatin using the electron probe microanalysis method. The electron probe microanalysis is one of the most popular methods of quantitative and semi-quantitative nondestructive elemental analysis. Spectrometric profiles are described for defining the composition of carboxymethylcellul...

  13. A mass spectrometry-based hybrid method for structural modelling of protein complexes

    OpenAIRE

    Politis, Argyris; Stengel, Florian; Hall, Zoe; Hernández, Helena; Leitner, Alexander; Walzthoeni, Thomas; Robinson, Carol V.; Aebersold, Ruedi

    2014-01-01

    We describe a method that integrates data derived from different mass spectrometric (MS) techniques with a modelling strategy for structural characterization of protein assemblies. We encoded structural data derived from native MS, bottom-up proteomics, ion mobility-MS and chemical cross-linking MS into modelling restraints to compute the most likely structure of a protein assembly. We used the method to generate near-native models for three known structures and characterized an assembly inte...

  14. Electrothermal atomic absorption spectrometric determination of total and hexavalent chromium in atmospheric aerosols

    International Nuclear Information System (INIS)

    A method was developed which allow separate determination of Cr(VI) and total Cr from the same minute sample of atmospheric aerosols. Cr(VI) was leached was with 0.1 M Na2CO3 and the total Cr concentrations were determined after acid digestion. The method was validated by the analysis of certified reference materials, CRM 545, Mess-3 and Pacs-2 with good agreement between certified and found values. Cr concentrations in air samples taken around the chromium smelter show concentrations that exceed the maximum allowed levels in 8 h with higher values closer to the smelter. The limit of detection (LOD) of the method for Cr(VI) determination in air samples was found to be 0.2 ng m-3, i.e. lower than offered by the commonly preferred spectrophotometric and colorimetric techniques

  15. Simultaneous kinetic spectrometric determination of three flavonoid antioxidants in fruit with the aid of chemometrics

    Science.gov (United States)

    Sun, Ruiling; Wang, Yong; Ni, Yongnian; Kokot, Serge

    2014-03-01

    A simple, inexpensive and sensitive kinetic spectrophotometric method was developed for the simultaneous determination of three anti-carcinogenic flavonoids: catechin, quercetin and naringenin, in fruit samples. A yellow chelate product was produced in the presence neocuproine and Cu(I) - a reduction product of the reaction between the flavonoids with Cu(II), and this enabled the quantitative measurements with UV-vis spectrophotometry. The overlapping spectra obtained, were resolved with chemometrics calibration models, and the best performing method was the fast independent component analysis (fast-ICA/PCR (Principal component regression)); the limits of detection were 0.075, 0.057 and 0.063 mg L-1 for catechin, quercetin and naringenin, respectively. The novel method was found to outperform significantly the common HPLC procedure.

  16. Photoelectrostimulated passivation of spectrometric Cd1–xZnxTe-detectors

    Directory of Open Access Journals (Sweden)

    Fedorenko O. A.

    2010-03-01

    Full Text Available A new physical method of Cd1–xZnxTe-detector’s treatment – photoelectrostimulated passivation is developed. In its frames, oxidation of the sample followed by the formation of high-resistance oxide layer on the surface occurs at simultaneous action of both intense light radiation and electric field. It is shown that the method is easily realized and provides the obtaining of thick high-resistance oxide films, that essentially increases the surface electrical resistance of Cd1–xZnxTe-samples and diminishes leakage currents in them.

  17. Preprocessing of Tandem Mass Spectrometric Data Based on Decision Tree Classification

    Institute of Scientific and Technical Information of China (English)

    Jing-Fen Zhang; Si-Min He; Jin-Jin Cai; Xing-Jun Cao; Rui-Xiang Sun; Yan Fu; Rong Zeng; Wen Gao

    2005-01-01

    In this study, we present a preprocessing method for quadrupole time-of-flight(Q-TOF) tandem mass spectra to increase the accuracy of database searching for peptide (protein) identification. Based on the natural isotopic information inherent in tandem mass spectra, we construct a decision tree after feature selection to classify the noise and ion peaks in tandem spectra. Furthermore, we recognize overlapping peaks to find the monoisotopic masses of ions for the following identification process. The experimental results show that this preprocessing method increases the search speed and the reliability of peptide identification.

  18. X-ray spectrometric technique for measuring porcelain-metal adherence

    International Nuclear Information System (INIS)

    This study demonstrated a correlation between silicon x-ray counts and area fractions of adherent porcelain as determined by point-counting. This correlation has allowed a method to be devised for measuring area fractions of porcelain adherent to porcelain-fused-to-metal (PFM) fracture surfaces. The described method, after controlled destruction of the porcelain mass, uses silicon x-rays excited by the electron beam in a scanning electron microscope. Under the conditions employed in these studies, the x-ray technique has shown that this gold alloy retains more porcelain than does either of two particular nickel-chromium alloys

  19. Autonomous long-term gamma-spectrometric monitoring of submarine groundwater discharge trends in Hawaii

    Czech Academy of Sciences Publication Activity Database

    Dulai, H.; Kameník, Jan; Waters, C. A.; Kennedy, J.; Babinec, J.; Jolly, J.; Williamson, M.

    2016-01-01

    Roč. 307, č. 3 (2016), s. 1865-1870. ISSN 0236-5731. [10th International Conference on Methods and Applications of Radioanalytical Chemistry (MARC). Kailua Kona, 12.04.2015-17.04.2015] Institutional support: RVO:61389005 Keywords : submarine groundwater discharge * long-term SGD monitoring * underwater gammaspectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 1.034, year: 2014

  20. Determination of rhenium in molybdenite by X-ray fluorescence. A combined chemical-spectrometric technique

    Science.gov (United States)

    Solt, M.W.; Wahlberg, J.S.; Myers, A.T.

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 ??g of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. ?? 1969.