Preconcentration and Determination of Trace Nickel and Cobalt in Milk-Based Samples by Ultrasound-Assisted Cloud Point Extraction Coupled with Flame Atomic Absorption Spectrometry.

In this study, ultrasound-assisted cloud point extraction (UA-CPE) method was developed for the determination of Ni(II) and Co(II) in milk-based products. After extraction and preconcentration, the Ni(II) and Co(II) contents of samples were determined by flame atomic absorption spectrometry (FAAS). After their complexation with hydroxy naphthol blue (HNB) in the presence of cationic surfactant, CTAB at pH 4.0, the Ni(II) and Co(II) were taken within the micellar phase of nonionic surfactant, TX-114. The micellar phase containing the analytes were diluted to a volume of 0.7 mL with 1.0-mol/L HNO in ethanol to reduce its viscosity and to facilitate sample treatment and then was analyzed by FAAS. The various analytical parameters affecting UA-CPE efficiency were investigated. The analytical features obtained after optimization are as follows: limits of detection are 0.56 and 0.78 μg/L; sensitivity enhancement factors are 48.6 and 53.9; the calibration curves were linear 3-180 and 2-160 μg/L for Co(II) and Ni(II), respectively, after preconcentration of 50-fold. The precision (as RSD%) between 1.8-3.6% and 2.2-3.8% (25 and 100 μg/L, n = 5) for Ni(II) and Co(II), respectively. The accuracy was statistically verified by analysis of two certified reference material samples (CRMs), including recovery studies after spiking. The method was applied to the analysis of milk-based samples with satisfied results.