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Gas chromatographic determination of alkali metal O,O-diethyl phosphorodithioate present in trace amounts

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Summary

A gas Chromatographic determination of traces of alkali metal O,O-diethyl phosphorodithioates is described. The salts were converted into a volatile derivative by alkylation with diazomethane. The product was identified by gas chromatography-mass spectrometry. With aqueous samples a linear relationship of peak height to amount of salt was obtained in the range 0.04–1 ng and for urine samples a calibration curve was constructed. The detection limit (signal to noise ratio 4/1) was 40 pg of salt. The procedure was successfully used for monitoring phosalone absorption by occupationally exposed persons.

Zusammenfassung

Eine gaschromatographische Bestimmung von Spuren Alkalisalz des Diäthyldithiophosphorsäureesters wurde beschrieben. Die Salze wurden durch Alkylieren mit Diazomethan in ein flüchtiges Derivat übergeführt. Dessen Identifizierung erfolgte mittels eines gaschromatographisch-massenspektrometrischen Systems. In Wasserproben wurde ein lineares Verhältnis der Peakhöhen und der Salzmenge festgestellt und für Urinproben wurde eine Eichkurve ermittelt. Die Nachweisgrenze (Signal zu Rausch 4∶1) wurde bei 40 pg Salz festgestellt. Die Methode wurde für die Kontrolle der Absorption von Phosalon bei beruflich exponierten Personen erfolgreich angewendet.

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Authors and Affiliations

  1. Institute for Medical Research and Occupational Health, Zagreb, Yugoslavia

    V. Drevenkar, M. Stipcević, B. Štengl & Z. Štefanac

Authors
  1. V. Drevenkar
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  2. M. Stipcević
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  3. B. Štengl
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  4. Z. Štefanac
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Drevenkar, V., Stipcević, M., Štengl, B. et al. Gas chromatographic determination of alkali metal O,O-diethyl phosphorodithioate present in trace amounts. Mikrochim Acta 71, 385–394 (1979). https://doi.org/10.1007/BF01197410

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  • DOI: https://doi.org/10.1007/BF01197410

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