Publications by authors named "Shona McSheehy"

Maturation of inductively coupled plasma-mass spectrometry (ICP-MS) in terms of size, reliability, and cost has had a significant impact on its consideration as a viable detector for gas chromatography. Its generally excellent sensitivity for those elements it can measure has been a contributing factor. A method for sulfur speciation in various hydrocarbon products is investigated, as well as sulfur and metal hydride contaminants in high purity hydrocarbon feed stocks.

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A new selenized yeast reference material (SELM-1) produced by the Institute for National Measurement Standards, National Research Council of Canada (INMS, NRC) certified for total selenium (2,059+/-64 mg kg(-1)), methionine (Met, 5,758+/-277 mg kg(-1)) and selenomethionine (SeMet, 3,431+/-157 mg kg(-1)) content is described. The +/-value represents an expanded uncertainty with a coverage factor of 2. SeMet and Met amount contents were established following a methanesulfonic acid digestion of the yeast using GC-MS and LC-MS quantitation.

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Selenomethionine (SeMet) and methionine (Met), liberated by acid hydrolysis of selenium-enriched yeast, were quantified by liquid chromatography-mass spectrometry (LC/MS) using standard additions calibrations as well as isotope dilution (ID) based on species-specific (13)C-enriched spikes. LC inductively coupled plasma mass spectrometry (ICPMS) was also employed for the quantification of SeMet, and (74)Se-enriched SeMet was used for ID calibration. The results were evaluated to ascertain the feasibility of using these methods in a campaign to certify selenized yeast.

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Fourteen extraction methods commonly cited in the literature were evaluated for the quantitation of methionine (Met) and selenomethionine (SeMet) in a yeast candidate certified reference material (CRM). Species specific isotope dilution (ID) gas chromatography-mass spectrometry (GC-MS) was utilized to effectively compensate for potential errors, such as losses during derivatization and clean up steps. Despite different extraction methods, the same derivatization procedure using methyl chloroformate was applied with a single exception, which was based on digestion with cyanogen bromide with 2% SnCl2 in 0.

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The identification of water-soluble arsenic species in a kidney of the Tridacna clam by electrospray quadrupole/time-of-flight mass spectrometry (ES Q-TOF MS) was investigated. The species were isolated by three-dimensional LC (size exclusion-anion exchange-cation exchange); the elution of arsenic was monitored by ICPMS. The average accuracy and precision of the molecular mass measurements, studied for a number of organoarsenic standards, were 22 (negative bias) and 15 ppm, respectively.

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An analytical strategy was developed for the characterization of arsenic species in a Laminaria algae. The approach was based on multidimensional liquid chromatography (LC) including sample extract cleanup by size-exclusion LC, separation of arsenic species by anion-exchange LC, verification of the chromatographic purity of arsenic-containing fractions, and their further purification, if necessary, by reversed-phase (RP) HPLC. The complementarity of ICP MS, used as the chromatographic detector, and ES MS/MS, employed for the identification of the peaks observed, was demonstrated.

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A three-dimensional liquid chromatographic purification protocol based on sequential size-exclusion, anion-exchange and cation-exchange separation mechanisms was developed for the mapping of seleno compounds in aqueous yeast extracts. The method allowed the demonstration of the presence of more than 30 different seleno compounds. Semi-preparative size-exclusion and anion-exchange chromatography were optimized for maximum resolution using electrospray-compatible buffers in order to purify the compounds for mass spectrometric analysis.

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