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

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

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 meth...

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Bibliographic Details
Published in:Accreditation and quality assurance Vol. 10; no. 8; pp. 444 - 451
Main Authors: SALTIENE, Zydre, JATULIENE, Natalija, SALKAUSKAS, Mudis, BRUKSTIENE, Dalva, RUZGYTE, Asta, TARASEVICIUTE, Ausra, KALIBATAS, Julius
Format: Journal Article
Language:English
Published: Heidelberg Springer 01-12-2005
Berlin Springer Nature B.V
Subjects:
Alcohol
Analytical chemistry
Calibration
Chemistry
Chromatographic methods and physical methods associated with chromatography
Exact sciences and technology
High performance liquid chromatography
Mathematical analysis
Other chromatographic methods
Solid phases
Standard deviation
Uncertainty
Urine
Germany
Urine
Solid phase extraction
Uncertainty
Biomarker
Enzyme
HPLC chromatography
Polycyclic aromatic compound
Chemical enrichment
Hydrolysis
Sample preparation
Detection limit
1-Hydroxypyrene
Standard curve
Level-dependent uncertainty
PAHS
Quantitative analysis
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Summary: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.
ISSN:0949-1775
1432-0517
DOI:10.1007/s00769-005-0001-z