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Estimation scheme for level-dependent uncertainty of analytical result: application for determination of 1-hydroxypyrene in urine

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Abstract

The estimation scheme of uncertainty of determination of 1-hydroxypyrene (1-OHP) in urine was developed analysing the main stages of the analytical procedure: (1) preparation of 1-OHP standards, (2) creation of the calibration curve for the high performance liquid chromatography (HPLC) analysis method with the evaluation of recovery, (3) measuring procedure of aliquot of urine, (4) adjusting the pH of aliquot and hydrolysis with enzyme, (5) solid phase extraction, (6) concentration of the extract, (7) injection of the extract to chromatograph and analysing by the HPLC method, (8) calculation of 1-OHP mass from the calibration curve, (9) calculation of 1-OHP concentration in urine. The evaluation of the uncertainty is based on quantification of individual components. Combined uncertainty was calculated using the law of propagation of uncertainties according to the EURACHEM/CITAC guidelines. Level dependence of the uncertainty arises from the calibration curve.

The limits of detection and quantification were found to be equal to 0.03 and 0.1 ng/mL, respectively. The calculated expanded level-dependent uncertainty covers 47–27–25% within the concentration range 0.03–0.1–0.4 ng/mL with the materials and equipment used. These parameters could easily be recalculated according to the proposed scheme if there are some changes in the analysis procedure.

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Acknowledgements

The authors thank Violeta Dumskiene for technical assistance and Irene and Andrew Read for editing language and grammar.

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Authors and Affiliations

  1. Institute of Hygiene of Lithuanian Ministry of Health, Didžioji 22, LT-01128, Vilnius, Lithuania

    Žydrė Šaltienė, Natalija Jatulienė, Daiva Brukštienė, Aušra Tarasevičiūtė & Julius Kalibatas

  2. Lithuanian Chemical Society, A. Goštauto 9, LT-01108, Vilnius, Lithuania

    Mudis Šalkauskas

  3. Institute of Chemistry, A. Goštauto Str. 9, LT-01108, Vilnius, Lithuania

    Asta Ruzgytė

Authors
  1. Žydrė Šaltienė
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  2. Natalija Jatulienė
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  3. Mudis Šalkauskas
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  4. Daiva Brukštienė
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  5. Asta Ruzgytė
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  6. Aušra Tarasevičiūtė
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  7. Julius Kalibatas
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Correspondence to Žydrė Šaltienė.

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Šaltienė, Ž., Jatulienė, N., Šalkauskas, M. et al. Estimation scheme for level-dependent uncertainty of analytical result: application for determination of 1-hydroxypyrene in urine. Accred Qual Assur 10, 444–451 (2005). https://doi.org/10.1007/s00769-005-0001-z

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  • DOI: https://doi.org/10.1007/s00769-005-0001-z

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