A stability-indicating liquid chromatographic (LC) method was developed for the determination of posaconazole in bulk. Chromatographic separation was achieved using an isocratic elution in a reversed-phase system, with a mobile phase composed of methanol-water (75:25, v/v), at 1.0 mL min−1 flow. Samples were exposed to degradation under thermal, oxidative and acid/basic conditions, and no interference in the analysis was observed. System suitability was evaluated and results were satisfactory (N = 4,900.00 tailing factor 1.04; RSD between injections = 0.65). The retention time of posaconazole was about 8.5 min and the method was validated within the concentration range 5–60 μg mL−1 (r = 0.9996). Adequate results were obtained for repeatability (RSD % = 0.86–1.22), inter-day precision (RSD % = 1.21) and accuracy (98.13% mean recovery). Robustness was also determined to be satisfactory after evaluation. The proposed method was successfully applied to posaconazole bulk quantification, showing the method is useful for determination of the drug in routine analysis.
This study assessed the limnology from the Medium Uruguay River Basin in Uruguaiana, Brazil, with a focus on the concentration of heavy metals (Cd, Cu, and Mn), to assess the toxicological potential (cytotoxicity and genotoxicity) for humans using as biological matrix of study human leukocyte cells. The conductivity, resistivity, and dissolved O 2 levels exceeded the limits recommended by the National Environmental Council (Conselho Nacional do Meio Ambiente-CONAMA). The percentage of non-viable human leukocyte cells exposed to water samples was approximately 20% higher than that of the negative control (<3%), but similar to the positive control. The DNA damage index was high for all heavy metal concentrations assayed when compared to the negative control 12±2.96, p < 0.0001, with a range of 155.66±23.89 to 194.33±23.23, but similar to the positive control (210.62±27.48). Moreover, the leukocyte degeneration index was higher in all samples containing heavy metals than in the negative control (4%), which demonstrates to be due the presence of Cu (11.8-12.5%), Cd (13-15.6%), and Mn (15.6-22.5%). Taken together, our results show that the quality from water samples analyzed is below than recommended by CONAMA and offers risk of contamination by heavy metals for the general population.
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