This work focuses on the development, validation and application of an analytical method for the determination of twenty organochlorine pesticides (OCPs) in human tissues using salting-out liquid–liquid extraction and dispersive liquid–liquid microextraction for sample preparation and gas chromatography–mass spectrometry to analyze the obtained extracts. Measurement of the concentration levels of these toxics in tissues can be used to assess the risk of the population to exposure. The linearity of the proposed method was verified in the 10–1,000 ng/g range. The sensitivity was evaluated calculating the limits of detection (LODs) for 20 OCPs (α-, β-, γ- and δ-hexachlorocyclohexane (HCH), α- and β-endosulfan, endosulfan sulfate, aldrin, dieldrin, endrin, endrin ketone, endrin aldehyde, α- and γ-chlordane, 4,4′-dichlorodiphenyltrichloroethane, 4,4′-dichlorodiphenyldichloroethylene (DDE), 4,4′-dichlorodiphenyldichloroethane, heptachlor, heptachlor epoxide and methoxychlor), most of them being found between 1.0 and 16 ng/g. The intra- and interday precisions were <12% for relative standard deviation values. The accuracy of the method was evaluated by recovery studies, which gave recovery percentages in the 85–109% range. Seven different tissues (liver, kidney, heart, spleen, lung, brain and abdominal fat) from eight autopsies were analyzed, and only three cases were seen to have β-HCH and 4,4′-DDE in abdominal fat, while 4,4′-DDE was also detected in the heart of one case. The rest of the samples were free of the studied OCPs at least above the corresponding LODs.
A study of the transient potential signals obtained with a cation-selective electrode based on an ion-exchanger was carried out for solutions of the following individual cations at different concentrations: H+, Li+, Na+, K+, Rb+, Mg2+, Ca2+, choline (Ch+), acetylcholine (AcCh+), and procaine (Pr+). Three different general types of transient signals were distinguished depending on the value of the selectivity coefficient of the corresponding ion. A principal component analysis (PCA) was performed on the signals, finding that the qualitative identification of the corresponding ion from the scores of two principal components is possible. The study was extended to the transient signals of solutions containing an analyte in the presence of an interfering ion. The PCA of the corresponding signal allows for the detection of the presence of interfering ions, thus avoiding biased results in the determination of the analyte. Moreover, the two principal components of the transient signals obtained for each of the ions at different concentrations allow for the construction of calibration graphs for the quantitative determination of the corresponding ion. All the transient signals obtained experimentally in this work can be reconstructed accurately from principal components and their corresponding scores.
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