3.3.1. Olive samples
A representative 20 g portion of olives (including the seed of the crop) previously homogenized was weighed and transferred to a glass mortar, where it was fortified homogenously with 2 ml of the bidistilled water because of its solubilizing effect of paraquat [36]. The mixture was then gently blended in the mortar for 30 min to assess the homogeneity of the sample. The mixture samples were used after filtration step, to prepare the supporting electrolyte (by adding 0.1 mol L−1 Na2SO4) and corresponding analytical curves were again obtained applying for SWASV experiments. The recovery studies were realized by adding an appropriate volume of paraquat standard solution (1×10−5 mol L−1) to electrochemical cell. The recovery results obtained, in triplicate, were related to the interference effects of the constituents of each sample (Table 3). The statistical calculations for the assay results showed suitable precision of the proposed voltammetric method. There were no significant differences between the calculated and added concentrations at the 95% confidence level and within an acceptable range of error. The results of relative standard deviations (5.9%) and the recovery percentage (94.4%) that were obtained for peak 2, were considered satisfactory compared to those obtained using other analytical methods, considering that neither the extraction or preparation stages of the samples are necessary in the proposed methodology. The slight decrease in the values of the recovery reflects an electrochemical process involving depression due to competitive effects between analytes, fouling of electrode or passivation of analyte response.
3.3.1 3.3.1. Olive samples
A representative 20 g portion of olives (including the seed of the crop) previously homogenized was weighed and transferred to a glass mortar, where it was fortified homogenously with 2 ml of the bidistilled water because of its solubilizing effect of paraquat [36]. The mixture was then gently blended in the mortar for 30 min to assess the homogeneity of the sample. The mixture samples were used after filtration step, to prepare the supporting electrolyte (by adding 0.1 mol L−1 Na2SO4) and corresponding analytical curves were again obtained applying for SWASV experiments. The recovery studies were realized by adding an appropriate volume of paraquat standard solution (1×10−5 mol L−1) to electrochemical cell. The recovery results obtained, in triplicate, were related to the interference effects of the constituents of each sample (Table 3). The statistical calculations for the assay results showed suitable precision of the proposed voltammetric method. There were no significant differences between the calculated and added concentrations at the 95% confidence level and within an acceptable range of error. The results of relative standard deviations (5.9%) and the recovery percentage (94.4%) that were obtained for peak 2, were considered satisfactory compared to those obtained using other analytical methods, considering that neither the extraction or preparation stages of the samples are necessary in the proposed methodology. The slight decrease in the values of the recovery reflects an electrochemical process involving depression due to competitive effects between analytes, fouling of electrode or passivation of analyte response.
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