title: Optimization and Validation of an ETAAS Method for the Determination of Nickel in Postmortem Material.
abstract: In this article, optimization and validation of a procedure for the determination of total nickel in wet digested samples of human body tissues (internal organs) for forensic toxicological purposes are presented. Four experimental setups of the electrothermal atomic absorption spectrometry (ETAAS) using a Solaar MQZe (Thermo Electron Co.) were compared, using the following (i) no modifier, (ii) magnesium nitrate, (iii) palladium nitrate and (iv) magnesium nitrate and ammonium dihydrogen phosphate mixture as chemical modifiers. It was ascertained that the ETAAS without any modifier with 1,300/2,400°C as the pyrolysis and atomization temperatures, respectively, can be used to determine total nickel at reference levels in biological materials as well as its levels found in chronic or acute poisonings. The method developed was validated, obtaining a linear range of calibration from 0.76 to 15.0 μg/L, limit of detection at 0.23 µg/L, limit of quantification at 0.76 µg/L, precision (as relative standard deviation) up to 10% and accuracy of 97.1% for the analysis of certified material (SRM 1577c Bovine Liver) and within a range from 99.2 to 109.9% for the recovery of fortified liver samples.
authors: Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland.
authors: Danuta
authors: D
authors: Dudek-Adamska
authors: Institute of Forensic Research, Westerplatte 9, 31-033 Kraków, Poland tlech@ies.krakow.pl.
authors: Teresa
authors: T
authors: Lech
authors: Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland.
authors: Paweł
authors: P
authors: Kościelniak
mesh_terms: D000818:Animals; D001344:Autopsy; D001923:Brain Chemistry; D002138:Calibration; D002417:Cattle; D053593:Forensic Toxicology / Q000379:methods*; D006321:Heart; D006358:Hot Temperature; D006801:Humans; D008099:Liver / Q000737:chemistry*; D008168:Lung / Q000737:chemistry*; D017616:Magnesium Compounds / Q000032:analysis; D009206:Myocardium / Q000737:chemistry*; D009532:Nickel / Q000032:analysis*; D009566:Nitrates / Q000032:analysis; D010165:Palladium / Q000032:analysis; D010710:Phosphates / Q000032:analysis; D015203:Reproducibility of Results; D013054:Spectrophotometry, Atomic / Q000379:methods; D013270:Stomach / Q000737:chemistry*
chemical_list: D017616:Magnesium Compounds; D009566:Nitrates; D010710:Phosphates; C024788:ammonium phosphate; C090639:palladium nitrate; D010165:Palladium; C018330:magnesium nitrate; D009532:Nickel