In-house method validation : Application in arsenic analysis

作者: Scheilla VC de Souza , Carlos T Pinto , Roberto G Junqueira , None

DOI: 10.1016/J.JFCA.2006.09.002

关键词:

摘要: Abstract A detailed procedure for in-house method validation was proposed and applied to the of a determination arsenic in bovine liver. Linearity matrix effects were assessed by solvent matrix-matched curves. Data fitted ordinary least squares (OLSM). Violations assumptions underlying OLSM residuals (normality, independence homoscedasticity) evaluated. F-tests undertaken check adjustment model evaluation regression lack fit significances. The slopes interceptions compared significant differences t-test. demonstrated not observed between 0.5 8 ng mL−1. Selectivity, trueness, precision experimental limits established assays with blanks spiked samples. Recovery (means 88.9–99.9%) calculated analysis variance carried out estimate standard deviation under repeatability (3.7–7.2%) within-reproducibility (3.7–7.3%) conditions. spiking experiments indicated no trueness. Experimental detection quantification 15 30 μg kg−1, respectively. found be suitable respect efficiency parameters, ease application cost-benefits.

参考文章(24)
Dimiter L. Tsalev, Vapor generation or electrothermal atomic absorption spectrometry? — Both! Spectrochimica Acta Part B: Atomic Spectroscopy. ,vol. 55, pp. 917- 933 ,(2000) , 10.1016/S0584-8547(00)00202-0
Vic Barnett, Toby Lewis, Outliers in Statistical Data ,(1978)
Frank E. Grubbs, Procedures for Detecting Outlying Observations in Samples Technometrics. ,vol. 11, pp. 1- 21 ,(1969) , 10.1080/00401706.1969.10490657
Dang Q. Hung, Olga Nekrassova, Richard G. Compton, Analytical methods for inorganic arsenic in water: a review. Talanta. ,vol. 64, pp. 269- 277 ,(2004) , 10.1016/J.TALANTA.2004.01.027
William. Horwitz, Evaluation of analytical methods used for regulation of foods and drugs Analytical Chemistry. ,vol. 54, pp. 67- 76 ,(1982) , 10.1021/AC00238A002
J. Durbin, G. S. Watson, Testing for Serial Correlation in Least Squares Regression. II Springer Series in Statistics. ,vol. 38, pp. 260- 266 ,(1992) , 10.1007/978-1-4612-4380-9_21
Shona McSheehy, Joanna Szpunar, Roberto Morabito, Philippe Quevauviller, The speciation of arsenic in biological tissues and the certification of reference materials for quality control Trends in Analytical Chemistry. ,vol. 22, pp. 191- 209 ,(2003) , 10.1016/S0165-9936(03)00404-7
J. Růžička, J.W.B. Stewart, Flow Injection Analysis Analytica Chimica Acta. ,vol. 79, pp. 79- 91 ,(1976) , 10.1016/S0003-2670(00)89421-0