DLLME-SFO-GC-MS procedure for the determination of 10 organochlorine pesticides in water and remediation using magnetite nanoparticles.

There exists a high demand for fast, simple, and reliable methodologies for determining the presence of organochlorine pesticides (OCPs) on environmental samples. Moreover, the toxicity and accumulation of potential OCPs in several environments have led to the development of technologies that achieve their removal from contaminated waters. In this study, a novel method combining a dispersive liquid-liquid microextraction procedure based on the solidification of floating organic drop is developed and validated for the extraction, preconcentration, and determination of 10 OCPs: α-BHC, p,p'-DDE, δ-BHC, dieldrin, p,p'-DDT, endosulfan I, endosulfan sulfate, heptachlor, heptachlor epoxide (isomer B), and methoxychlor in water samples. The results show that the calibration curves were linear for all the studied compounds, and the coefficients of correlation higher than 0.99. The variation coefficient for precision and accuracy was lower than 10%, and the accuracy ranged from 93 to 105%. Low limit of detection and limit of quantification values ranging from 0.06-3.00 ng mL-1 and 0.20-10 ng mL-1 were obtained, respectively. The capability of the proposed method was confirmed using an analysis of the water samples before and after the degradation process; this was achieved by employing nanomaterials, while performing an analysis of 160 real samples that were sourced from a Brazilian river. A cobalt-doped magnetite was applied for the environmental remediation of the studied compounds, and it was verified that the novel material has the potential to be used in environmental remediation with a degradation efficiency exceeding 80% for the majority of the studied compounds.

Identification of species of the Euterpe genus by rare earth elements using inductively coupled plasma mass spectrometry and linear discriminant analysis.

The açaí (Euterpe oleracea Mart.) and juçara (Euterpe edulis Mart.) produce similar fruits which are rich in energy, minerals, vitamins and natural compounds with antioxidant and anti-inflammatory properties. Although the drink obtained from these species is similar, it is important to develop tools to establish the identity of the fruit species and growing regions. To assess claims of origin and for other purposes, we use multivariate analysis to investigate the differentiation of açaí and juçara fruits based on rare earth element (REE) content determined by Inductively Coupled Plasma Mass Spectrometry. REE content, in particular Sm, Th, La, Pr, Gd, and especially Ce and Nd varied between species. PCA analysis was not efficient in differentiating açaí from juçara fruit samples. In contrast, LDA analysis permitted a correct differentiation between species with a predictive ability of 83.3%. The methodology that we have applied confirms that REE can be used to differentiate between açaí and juçara fruit samples and to identify their origin.

Speciation of Sb(III) and Sb(V) in meglumine antimoniate pharmaceutical formulations by PSA using carbon nanotube electrode.

A new and simple electroanalytical method for speciation of Sb(III) and Sb(V) in pharmaceutical formulation by potentiometric stripping analysis (PSA) using a multiwall carbon nanotube paste electrode was developed. All instrumental and chemical parameters influencing the performance of the method were carefully assessed and optimized. Trivalent antimony was determined in acid medium (pH 3.6) under the optimized condition (deposition potential of -0.7 V, deposition time of 180 s, ionic strength of 0.3M and oxidant mercury concentration of 10 mg l(-1)). Total antimony was determined after quantitative reduction of Sb(V) with l-cysteine (1.5%, w/v) and its concentration was calculated from difference between the total antimony and Sb(III). The developed method provided two distinct linear calibration one ranging from 10 up to 50 microg l(-1) and other from 100 up to 800 microg l(-1) with respective correlation coefficient of 0.9978 and 0.9993, presenting a detection limit of 6.2 microg l(-1). Repeatability for the six independent samples expressed in terms of relative standard deviation was found to be 3.01 and 1.39% for 40.0 and 300.0 microg l(-1) antimony concentration, respectively. Results on the effect of foreign substances [Al(III), Mg(II), Fe(III), Cd(II), Zn(II) and meglumine] on analytical signal of antimony showed no interference even using high content of foreign ions in the analyte:interferent ratio up to 1:100. The proposed method was successfully applied for the speciation of Sb(III) and Sb(V) in pharmaceutical formulation and the accuracy was assessed from addition and recovery tests as well as comparing with graphite furnace atomic absorption spectrometry (GF AAS) technique used as reference analytical method.

Simultaneous determination of zinc, cadmium and lead in environmental water samples by potentiometric stripping analysis (PSA) using multiwalled carbon nanotube electrode.

The present paper has focused on the potential application of multiwalled carbon nanotube for the development of a new, simple and highly selective electrochemical method for simultaneous Zn (II), Cd (II) and Pb (II) monitoring in water samples (lake and effluent waters), by using potentiometric stripping analysis (PSA). The electrochemical method is based on simultaneous preconcentration/reduction of metal ions onto a multiwall carbon nanotube electrode at -1.3V (versus Ag/AgCl(sat)) in 0.3 mol L(-1) acetate solution containing 15 mg L(-1) Hg (II) ions during 180s, followed by subsequent chemical stripping. The analytical curve for all analytes covered the linear range varying from 58.4 up to 646.2 microg L(-1) with correlation coefficients higher than 0.981. The limits of detection for Zn (II), Cd (II) and Pb (II) were found to be 28.0, 8.4 and 6.6 microg L(-1), while the relative standard deviation (RSD) at 352 microg L(-1) was 5.6, 7.1 and 5.6% (n=5), respectively. The behavior of the simultaneous determination in the presence of following ions Co (II), Cr (III) and Cu (II) was affected by using the analyte:interferent ratio 1:10. Therefore, by using standard addition method, Zn (II), Cd (II) and Pb (II) ions in lake and effluent water samples were determined after the spiking procedure and the results were successfully compared with those obtained by atomic absorption spectrometry (AAS). The obtained results suggest that the proposed method can be applied as a simple and efficient alternative for the simultaneous monitoring of heavy metals in water samples, according to those established requirements from environmental organizations. In addition, this method demonstrates the powerful application of carbon nanotubes in the field of potentiometric stripping analysis.