Estimation of the Main Sources of Uncertainty in Chromatographic Analysis: Determination of Biogenic Amines

نویسندگان

  • Roberto Romero
  • Domingo Gázquez
  • Mercedes Sánchez-Viñas
  • Luis Cuadros-Rodríguez
چکیده

Although the Eurachem guide shows some examples, analytical chemists frequently have regarded the estimation of uncertainty as too theoretical and not suitable for the estimation of uncertainties of complex chemical techniques. This is because identifying and quantifying all sources of uncertainty is difficult and laborious, for procedures consisting of numerous steps, many of which are not always clearly distinguishable. Analytical chromatographic procedures can be good examples of this situation, in which sources of uncertainty exist (5,6) such as sample handling, derivatization reaction, calibration function, matrix effect, and separation. Among the three approaches mentioned earlier for routine analysis, the combination of the bottom-up approach and the in-house validation data shows the most available information. Nevertheless, neither identification nor quantification of the uncertainty associated with the chemical factors of the method has been combined, so two sources related to the factors not controlled by the operator could be introduced. The first depends upon the chemical stages indicated in the procedure, and the second is associated with the chemical calibration process. This paper describes a general procedure for evaluating the uncertainty of the analytical results obtained in the determination of This article establishes the estimation of the uncertainty associated with the chromatographic determination of biogenic amines. The authors identify and estimate each source of uncertainty to establish the accuracy of results and to obtain a better understanding of the method. Thus, measurement uncertainty was split into two sections: uncertainty related to the working conditions, which considers the equipment used, and inherent uncertainty, which includes the chemical stages indicated in the procedure as well as calibration sources, taking into account the existence of the matrix effect. Recovery studies also were made to quantify the contribution of bias to the overall uncertainty. This parameter was calculated for the determination of biogenic amines in different types of samples. Estimation of the Main Sources of Uncertainty in Chromatographic Analysis: Determination of Biogenic Amines

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تاریخ انتشار 2004