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Paul A. D'Agostino Claude L. Chenier James R. Hancock Carmela R. Jackson Lepage 《Rapid communications in mass spectrometry : RCM》2007,21(4):543-549
Desorption electrospray ionisation mass spectrometry (DESI‐MS) was recently reported for the direct analysis of sample media without the need for additional sample handling. During the present study, direct analysis of solid‐phase microextraction (SPME) fibers by DESI‐MS/MS was evaluated with indoor office media that might be collected during a forensic investigation, including wall surfaces, office fabrics, paper products and Dacron swabs used for liquid sampling. Media spiked at the µg/g level with purified chemical warfare agents and a complex munitions grade sample of tabun, to simulate the quality of chemical warfare agent that might be used for terrorist purposes, were successfully analysed by DESI‐MS/MS. Sulfur mustard, a compound that has not been successfully analysed by electrospray mass spectrometry in the past, was also sampled using a SPME fiber and analysed for the first time by DESI‐MS/MS. Finally, the overall analytical approach involving SPME headspace sampling and DESI‐MS analysis was evaluated during a scenario‐based training live agent exercise. A sarin sample collected by the military was analysed and confirmed by DESI‐MS in a mobile laboratory under realistic field conditions. Copyright © 2007 Crown in the right of Canada. Published by John Wiley & Sons, Ltd. 相似文献
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Ivette M. Menndez‐Perdomo Jillian M. Hagel Peter J. Facchini 《Journal of mass spectrometry : JMS》2021,56(2)
Benzylisoquinoline alkaloids (BIAs) have profound implications on human health owing to their potent pharmacological properties. Notable naturally occurring BIAs are the narcotic analgesics morphine, the cough suppressant codeine, the potential anticancer drug noscapine, the muscle relaxant papaverine, and the antimicrobial sanguinarine, all of which are produced in opium poppy (Papaver somniferum). Thebaine, an intermediate in the biosynthesis of codeine and morphine, is used in the manufacture of semisynthetic opiates, including oxycodone and naloxone. As the only commercial source of pharmaceutical opiates, opium poppy has been the focus of considerable research to understand BIA metabolism in the plant. The elucidation of several BIA biosynthetic pathways has enabled the development of synthetic biology platforms aimed at the alternative commercial production of valuable phytochemicals in microorganisms. The detection and identification of BIA pathway products and intermediates in complex extracts is essential for the continuing advancement of research in plant specialized metabolism and microbial synthetic biology. Herein, we report the use of liquid chromatography coupled with linear trap quadrupole and high‐resolution Orbitrap multistage mass spectrometry to characterize 44 authentic BIAs using collision‐induced dissociation (CID), higher‐energy collisional dissociation (HCD), and pulsed Q collision‐induced dissociation (PQD) MS2 fragmentation, with MS2 CID followed by MS3 and MS4 fragmentation. Our deep library of diagnostic spectral data constitutes a valuable resource for BIAs identification. In addition, we identified 22 BIAs in opium poppy latex and roots extracts. 相似文献
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Speciation analysis of orthophosphate and myo‐inositol hexakisphosphate in soil‐ and plant‐related samples by high‐performance ion chromatography combined with inductively coupled plasma mass spectrometry
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Ariana Rugova Markus Puschenreiter Jakob Santner Lisa Fischer Stefan Neubauer Gunda Koellensperger Stephan Hann 《Journal of separation science》2014,37(14):1711-1719
A novel method based on high‐performance ion chromatography inductively coupled plasma mass spectrometry employing strong anion exchange chromatography with HNO3 gradient elution for simultaneous analysis of orthophosphate and myo‐inositol hexakisphosphate (IP6) in soil solution and plant extracts is presented. As inductively coupled plasma mass spectrometry analysis of phosphorus at m/z 31 is hampered by N‐based interferences, 31P was measured as 31P16O+ at m/z 47 employing dynamic reaction cell technique with O2 as reaction gas. Orthophosphate and IP6 were separated within a total chromatographic run‐time of 12 min revealing a limit of detection of 0.3 μmol/L. The coefficients of determination obtained in a working range of 1–100 and 1–30 μmol/L were 0.9991 for orthophosphate and 0.9968 for IP6, respectively. The method was successfully applied to extracts from three different soils as well as root and shoot extracts of Brassica napus L. The precision of three independently prepared soil extracts was in the range of 4–10% relative standard deviation for PO43? and 3–8% relative standard deviation for IP6. Soil adsorption/desorption kinetics for IP6/orthophosphate were performed for investigating the sorption behavior of the two P species in the experimental soils. 相似文献
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Thomas J. P. Smyth Virginia Rodríguez Robledo W. Franklin Smyth 《Rapid communications in mass spectrometry : RCM》2010,24(5):651-658
Oxazepam has been subjected to controlled degradation at 100°C for 3 h in 0.5 M HCl and 0.5 M NaOH. Following neutralisation of the degradation mixture and removal of salts by solid‐phase extraction (SPE), isocratic high‐performance liquid chromatography/mass spectrometry (HPLC/MS) using water/methanol (25:75 v/v) as the mobile phase was carried out using a flow diverter to collect fractions prior to their characterisation by electrospray ionisation multi‐stage mass spectrometry (ESI‐MSn) and proposal of the corresponding fragmentation patterns. The elemental compositions of the degradation products and their MS fragments were evaluated using electrospray ionisation quadrupole time‐of‐flight tandem mass spectrometry (ESI‐QTOF‐MS/MS) which was then used to support the proposed fragmentation patterns. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
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Prukała D Prukała W Koczorowski R Khmelinskii IV Sikorska E Sikorski M 《Rapid communications in mass spectrometry : RCM》2008,22(3):409-416
Electron ionisation (EI) mass spectra and electrospray ionisation (ESI) mass spectra at different cone voltages of a series of isomeric methyl- and dimethylalloxazines are discussed, and compared with those of lumichrome, and 1- and 3-methyllumichrome. Examination of ESI mass spectra taken at a higher cone voltage and the use of isotope-labelled methanol allow us to discuss the fragmentation pathways of [M+H]+ and [M-H](-) ions. The fragmentation pathways of all of the compounds and the characteristic fragment ions formed in EI-MS are compared with published data. The influence of methyl and dimethyl substituents in the benzene ring on the fragmentation pathways leading to the loss of 43 and 45 Da upon both electron and electrospray ionisation is described. 相似文献
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Four cation-exchange materials, possessing propanesulfonic acid ligands, for use in capillary electrochromatography were prepared from different commercially available 5-microm bare-silica particles ranging from 80 to 800 A in pore size. The performance of the materials was investigated at different compositions of the mobile phase (pH, ionic strength, and acetonitrile content) using tricyclic antidepressants and related quaternary ammonium analogues as test analytes. The wide-pore materials promoted pore flow, but this had no positive influence on the performance. The small-pore (highest surface area) particles gave, as could be expected, the best selectivity. 相似文献
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Igor Pavlovic Divyeshsinh T. Thakor Priv.‐Doz. Dr. Laurent Bigler Dr. Miranda S. C. Wilson Debabrata Laha Dr. Gabriel Schaaf Prof. Dr. Adolfo Saiardi Prof. Dr. Henning J. Jessen 《Angewandte Chemie (International ed. in English)》2015,54(33):9622-9626
Diphospho‐myo‐inositol phosphates (PP‐InsPy) are an important class of cellular messengers. Thus far, no method for the transport of PP‐InsPy into living cells is available. Owing to their high negative charge density, PP‐InsPy will not cross the cell membrane. A strategy to circumvent this issue involves the generation of precursors in which the negative charges are masked with biolabile groups. A PP‐InsPy prometabolite would require twelve to thirteen biolabile groups, which need to be cleaved by cellular enzymes to release the parent molecules. Such densely modified prometabolites of phosphate esters and anhydrides have never been reported to date. This study discloses the synthesis of such agents and an analysis of their metabolism in tissue homogenates by gel electrophoresis. The acetoxybenzyl‐protected system is capable of releasing 5‐PP‐InsP5 in mammalian cell/tissue homogenates within a few minutes and can be used to release 5‐PP‐InsP5 inside cells. These molecules will serve as a platform for the development of fundamental tools required to study PP‐InsPy physiology. 相似文献
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Atsushi Sudo Kohei Kaiba 《Journal of polymer science. Part A, Polymer chemistry》2019,57(12):1358-1364
A route from naturally occurring myo‐inositol to hydroxyl‐bearing polyurethanes has been developed. The diol prepared from the bis‐acetalization of myo‐inositol with 1,1‐dimethoxycyclohexane was reacted with a rigid diisocyanate, 1,3‐bis(isocyanatomethyl)cyclohexane to afford the corresponding polyurethane, of which glass transition temperature (Tg) was quite high as 192 °C. The polyurethane contains side chains inherited from the acetal moieties of the diol monomer and was treated with trifluoroacetic acid to hydrolyze the acetal moieties and afford the target polyurethane functionalized with hydroxyl groups. The presence of many hydroxyl groups in the side chains, which can form hydrogen bonds with each other, resulted in a high Tg, 186 °C. In addition, the hydroxyl groups were reacted with isocyanates to achieve further side‐chain modifications. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 1358–1364 相似文献
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The so-called imidazolines (2-alkyl-1-[ethylalkylamide]-2-imidazolines and 2-alkyl-1-ethylamine-2-imidazolines) are a group of surface-active compounds, complex mixtures of which are used by various industries as surfactants and corrosion inhibitors. Although their industrial synthesis was reported over 100 years ago, few methods for the determination of individual imidazolines in mixtures, including industrial matrices such as crude oils, have been reported. Here we demonstrate that spiking of crude oils with synthetic imidazolines followed by solid-phase extraction and liquid chromatography/electrospray ionisation multistage mass spectrometry (LC/ESI - MS(n)) allows an estimation of low (<10) parts per million concentrations of individual imidazolines in crude oils. Whilst non-optimised at present, the method is a significant advance and may prove useful not only for improving an understanding of the mechanisms of industrial imidazoline synthesis and for monitoring downhole and topside oilfield operations, but also for the determination of the fate of imidazoline-based oilfield corrosion inhibitors and surfactants in the environment. 相似文献
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Zambonin CG Losito I Palmisano F 《Rapid communications in mass spectrometry : RCM》2000,14(10):824-828
The main degradation by-products of the herbicide chlortoluron formed during water disinfection with HOCl/ClO(-) have been separated and identified by liquid chromatography/electrospray ionisation sequential mass spectrometry (LC/ESI-MS(n)). Chlorination and hydroxylation reactions seem to occur exclusively on the aromatic ring of chlortoluron, leading to by-products which show characteristic fragmentation patterns. Indeed, chlortoluron-like ESI spectra were always observed for chlorinated by-products, showing only a fragment at m/z 72. In contrast, hydroxylated and chloro/hydroxylated by-products gave a much more complex fragmentation pattern that could be elucidated by MS(n) (n = 1-4) experiments. A mechanistic scheme rationalising the observed fragmentation pattern is proposed and discussed. Copyright 2000 John Wiley & Sons, Ltd. 相似文献
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Doherty B Rodriguez V Leslie JC McClean S Smyth WF 《Rapid communications in mass spectrometry : RCM》2007,21(13):2031-2038
A tandem mass spectrometric investigation of the collision-induced dissociation of five commonly prescribed psychoactive pharmaceuticals, risperidone, sertraline, paroxetine, trimipramine, and mirtazapine, and their metabolites has been carried out. Quadrupole ion trap mass spectrometry was employed to generate tandem mass spectrometric (MS/MS) data of the compounds under investigation and structural assignments of product ions were supported by quadrupole time-of-flight mass spectrometry. These fragmentation studies were then utilised in the development of a liquid chromatographic method to identify the drugs and their metabolites in human hair and saliva samples, thus providing relevant profiling information. 相似文献
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Liquid chromatography with electrospray ionisation mass spectrometric detection of phenolic compounds from Olea europaea. 总被引:2,自引:0,他引:2
D Ryan K Robards P Prenzler D Jardine T Herlt M Antolovich 《Journal of chromatography. A》1999,855(2):529-537
The results demonstrate the potential of electrospray ionisation mass spectrometry for the specific detection of phenolic species in olives. Phenolic compounds were detected with greater sensitivity in the negative ion mode, but results from positive and negative ion modes were complementary with the positive ion mode showing structurally significant fragments. This is demonstrated by the identification of oleuropein and isomers of verbascoside. The structure of the latter were confirmed by retention, mass spectral and nuclear magnetic resonance data. These isomers have not previously been reported in olive. 相似文献
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Catalysts immobilised in ionic liquids have been analysed using electrospray ionisation ion trap mass spectrometry, which allows identification of the catalyst without contamination from the ionic liquid; additionally, a new ionic liquid containing the Monsanto catalyst as the anionic component, [Rh(CO)2I2]-, has been characterised using the same method. 相似文献
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同位素质谱与无机质谱分析 总被引:1,自引:0,他引:1
本文是《分析试验室》定期评述中“无机质谱分析”课题的第二篇评述文章,它增加了同位素质谱分析的内容,故将题目改为现今题目,它综述了1985年~1990年间同位素质谱和无机质谱的发展概况。其中包括同位素示踪、同位素稀释、火花源质谱、二次离子质谱、等离子体质谱等。内容以国内为主,也收集了少量代表学科先进水平的外国文献。 相似文献