Determination of thiocyanate in saliva by headspace gas chromatography-mass spectrometry, following a single-step aqueous derivatization with triethyloxonium tetrafluoroborate

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DOIResolve DOI: http://doi.org/10.1016/j.chroma.2015.04.040
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TypeArticle
Journal titleJournal of Chromatography A
ISSN0021-9673
Volume1400
Pages124130; # of pages: 7
SubjectThiocyanate; Saliva; Smokers and nonsmokers; Triethyloxonium tetrafluoroborate derivatization; GC/MS; Isotope dilution
AbstractA novel method for the determination of salivary thiocyanate is presented. Thiocyanate was converted into ethyl thiocyanate by single-step aqueous derivatization based on triethyloxonium tetrafluoroborate and measured by gas chromatography-mass spectrometry (15min runtime). The ethyl thiocyanate derivative is volatile and can be sampled from the headspace. The derivatization chemistry proposed allows for separation of the analyte from saliva matrix whose introduction in the measurement system is avoided. Quantitation of the analyte was obtained by isotope dilution, employing a 13C-enriched thiocyanate as internal standard. Technical details and fundamental aspects of derivatization chemistry and calibration strategy are presented.The method was validated by comparison with a standard method based on ion chromatography. The two independent methodologies produced results in agreement within 3%. Also a three level spike recovery test was carried out for validation purpose and quantitative recoveries were attained. The method is fast, simple, safe, and sensitive. Measurement of a 1. mL volume 50. ng/g of thiocyanate standard produced a signal-to-noise ratio of 250 for the analytical peak. This method is therefore suitable for ultra-trace determination of thiocyanate (low part-per-billion range). For the application described the full detection potential of the method was not required and the sample preparation presented has been designed for quantitation of saliva samples containing 1-400. μg/g of thiocyanate with a combined standard uncertainty of 2% relative for saliva samples containing 25. μg/g of thiocyanate. This method was applied for the determination of thiocyanate in human saliva samples.
Publication date
PublisherElsevier
LanguageEnglish
AffiliationNational Research Council Canada; Measurement Science and Standards
Peer reviewedYes
NPARC number21275825
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Record identifiera8070629-de69-4fa5-83d8-5d59b7dd0f78
Record created2015-07-14
Record modified2016-05-09
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