RESUMEN
Here, a novel nanohybrid material (Ag@CD@ANS) based on oat starch was produced, characterized, and applied to extract persistent organic pollutants in a shrimp sample. By the characterization experiments, Ag@CD@ANS was successfully synthesized. The functionalization of the material by 1,2-naphthoquinone-4-sulphonic acid (ANS) was confirmed using the infrared technique and CHN elemental analysis. The isotherm study showed that the material has a high adsorption capacity for the pesticides of interest (flutriafol, atrazine, heptachlor, DDT and bifenthrin) allowing their extraction from shrimp samples. The optimal condition for extraction was obtained using multivariate analysis. The nature of the elution solvent (hexane, methanol, acetonitrile) and the mass ratio between sample:adsorbent (1:1; 1:5 and 1:10) were the evaluated factors for extraction using Ag@CD@ANS and commercial adsorbents (neutral alumina, octadecyl, silica gel). From the multivariate analysis, it was observed that the optimal condition for pesticide extraction using Ag@CD@ANS was reached, using a 1:5 ratio (sample:adsorbent) and acetonitrile (10 mL) as elution solvent. For the commercial adsorbents, the optimal condition for pesticide extraction was reached, using a 1:3 ratio (sample:adsorbent), acetonitrile (10 mL) and neutral alumina as commercial adsorbent. Ag@CD@ANS efficiency was compared with an optimal commercial adsorbent (neutral alumina). No significant difference (p < 0.05) between neutral alumina and Ag@CD@ANS was observed. Recoveries ranging from 75 to 105 % with coefficients of variation ≤ 15 % (n = 3) were obtained using neutral alumina while using Ag@CD@ANS, recoveries ranging from 73 to 102 %, with coefficient of variation ≤ 13 % (n = 3) were obtained for the target pesticides. Limits of detection ranging from 0.5 to 1.0 µg Kg-1 and limits of quantification ranging from 1.6 to 3.3 µg Kg-1 were reached. The results demonstrated that Ag@CD@ANS can alternatively be used as a support for the extraction of persistent organic pollutants, having the advantage of being reusable for up to three cycles.
Asunto(s)
Contaminantes Orgánicos Persistentes , Plaguicidas , Solventes , Óxido de Aluminio , Acetonitrilos , Extracción en Fase Sólida/métodosRESUMEN
This paper reports the fabrication of polyester-toner (PT) electrophoresis microchips with improved analytical performance and extended lifetime. This has been achieved with a better understanding about the EOF generation and the influence of some parameters including the channel dimensions (width and depth), the injection mode, and the addition of organic solvent to the running buffer. The analytical performance of the PT devices was investigated using a capacitively coupled contactless conductivity detector and inorganic cations as model analytes. The proposed devices have exhibited EOF values of (3.4 ± 0.2) × 10(-4) cm(2) V(-1) s(-1) with good stability over 25 consecutive runs. It has been found that the EOF magnitude depends on the channel dimension, i.e. the wider the channel, the higher the EOF value. The separation efficiency for inorganic cations ranged from 13 000 to 50 000 plates/m. The LOD found for K(+) , Na(+) , and Li(+) were 4.2, 7.3, and 23 µM, respectively. In addition, the same PT device has been used by three consecutive days. Lately, due to improved analytical performance, it was carried out by the first time the detection of inorganic cations in real samples such as energetic drinks and pharmaceutical formulations.