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A novel method was developed for determination of trace amounts of lead in water and food samples. Solidified floating organic drop microextraction was used to preconcentrate the lead ion. After the analyte was complexed with 1-(2-pyridylazo)-2-naphthol, undecanol and acetonitrile were added as extraction and dispersive solvent, respectively. Variables such as pH, volumes of extraction and dispersive solvents, and concentration of chelating agent were optimized. Under the optimum conditions, the detection limit of Pb (II) was determined as 0.042 µg L−1 with an enrichment factor of 300. The relative standard deviation is <10%. Accuracy of the developed procedure was evaluated by the analysis of certified reference material of human hair (NCS DC 73347) and wastewater (SPS-WW2) with satisfactory results. The developed procedure was then successfully applied to biscuit and water samples for detection of Pb (II) ions. [ABSTRACT FROM AUTHOR]

[Display omitted] • AMGs were derived in situ in a single reaction vessel. • Developed LC-MS/MS method enabled rapid and practical AMG quantification. • Described derivatization is promising for guanidium-bearing compounds. • Frequency of AMG residues in honey samples (26.3%) was determined. Streptomycin (STR) and dihydrostreptomycin (DSTR) are the typically encountered aminoglycoside (AMG) residues in honey. For AMG analysis, studies in literature involve impractical and expensive applications such as ion-pairing chromatography, immunoassays, pre and post column derivatizations, or SPE approaches. Pretreatments of these methods are toilsome and costly. Herein, one-pot, aqueous in-situ derivatization method was presented as a superior protocol. Time and cost-efficient UHPLC-MS/MS method has been developed, and practical sample preparation was introduced. Satisfactory results were reported in method verification studies. The mean recovery values were 102.6% for STR and 101.3% for DSTR. Average values between 1.5% and 9.9% RSDs were found at intra and inter-day precisions. CCα (5.7 and 5.8 μg/kg) and CCβ (6.2 and 6.4 μg/kg) values were calculated for STR and DSTR respectively. AMG residues were found in 29 out of 110 analyzed samples using validated method. Described novelty enabled comprehensive analysis in an inexpensive and straightforward manner. [ABSTRACT FROM AUTHOR]

Cloud point extraction for the determination of copper(II) is proposed after the formation of a complex with sulfapyridylazo resorcinol (SPAR) and later measurement by flame atomic absorption spectrometry (FAAS) using Triton X-100 as a surfactant. The surfactant-rich phase was diluted with nitric acid in methanol, prior to FAAS measurement. Analytical parameters including pH, concentration of the chelating agent and surfactant, equilibration temperature and time were optimized. The effects of matrix ions on the recovery of copper ions were also studied. A detection limit of 1.64 μg l-1 along with an enrichment factor of 31 for Cu were achieved. The method was successfully applied to the determination of copper in tap water, stream water, rain water and a standard reference material. [ABSTRACT FROM AUTHOR]