RESUMEN
The present study aimed to evaluate the Strata-X® sorbent, commonly used in cartridges, through analysis by high-performance liquid chromatography coupled with mass spectrometry. Due to the different physical-chemical characteristics of the compounds, different conditions of chromatography and mass analysis were necessary. The developed methods were validated in terms of selectivity, linear range, linearity (coefficient of determination, r2), the limit of detection (LOD), the limit of quantification (LOQ), accuracy (recovery, %), and precision (RSD, %). The results allowed us to select efficient extraction methods, using methanol acidified to pH 2 with formic acid, to elute the herbicides 2,4-D and dicamba in both sorbent materials. Besides, the Strata-X® sorbent was efficient in the sorption of analytes; thus, we indicate it for potential use in air sampling as an alternative to XAD-2.
Asunto(s)
Dicamba , Herbicidas , Ácido 2,4-Diclorofenoxiacético , Cromatografía Líquida de Alta Presión , Dicamba/análisis , Herbicidas/análisis , Límite de DetecciónRESUMEN
A fully automated on-line system for monitoring the photocatalytic degradation of herbicides was developed using multisyringe flow injection analysis (MSFIA) coupled to a solid phase extraction (SPE) unit with UV detection. The calibration curves were linear in the concentration range of 100-1000 µg L(-1) for 3,6-dichloro-2-methoxybenzoic acid (dicamba) and 500-3000 µg L(-1) for 2,4-dichlorophenoxyacetic acid (2,4-D), while the detection limits were 30 and 135 µg L(-1) for dicamba and 2,4-D, respectively. The monitoring of the photocatalytic degradation (TiO2 anatase/UV 254 nm) of these two herbicides was performed by MSFIA-SPE system using a small sample volume (2 mL) in a fully automated approach. The degradation was assessed in ultrapure and drinking water with initial concentrations of 1000 and 2000 µg L(-1) for dicamba and 2,4-D, respectively. Degradation percentages of approximately 85% were obtained for both herbicides in ultrapure water after 45 min of photocatalytic treatment. A similar degradation efficiency in drinking water was observed for 2,4-D, whereas dicamba exhibited a lower degradation percentage (75%), which could be attributed to the presence of inorganic species in this kind of water.
Asunto(s)
Ácido 2,4-Diclorofenoxiacético/análisis , Dicamba/análisis , Monitoreo del Ambiente/métodos , Herbicidas/análisis , Sistemas en Línea , Contaminantes Químicos del Agua/análisis , Ácido 2,4-Diclorofenoxiacético/química , Dicamba/química , Monitoreo del Ambiente/instrumentación , Análisis de Inyección de Flujo/instrumentación , Análisis de Inyección de Flujo/métodos , Herbicidas/química , Sistemas en Línea/instrumentación , Fotólisis , Extracción en Fase Sólida/instrumentación , Extracción en Fase Sólida/métodos , Contaminantes Químicos del Agua/químicaRESUMEN
Simultaneous determination of three herbicides (dicamba, 2,4-D, and atrazine) has been achieved by on-line solid-phase extraction (SPE) coupled to multisyringe chromatography (MSC) with UV detection. The preconcentration conditions were optimized; a preconcentration flow rate of 0.5 mL min(-1) and elution at 0.8 mL min(-1) were the optimum conditions. A C(18) (8 mm i.d.) membrane extraction disk conditioned with 0.3 mol L(-1) HCl in 0.5% MeOH was used. A 3-mL sample was preconcentrated, then eluted with 0.43 mL 40:60 water-MeOH. A C(18) monolithic column (25 mm × 4.6 mm) was used for chromatographic separation. Separation of the three compounds was achieved in 10 min by use of 0.01% aqueous acetic acid-MeOH (60:40) as mobile phase at a flow rate of 0.8 mL min(-1). The limits of detection (LOD) were 13, 57, and 22 µg L(-1) for dicamba, 2,4-D, and atrazine, respectively. The sampling frequency was three analyses per hour, and each analysis consumed only 7.3 mL solvent. The method was applied to spiked water samples, and recovery between 85 and 112% was obtained. Recovery was significantly better than in the conventional HPLC-UV method. These results indicated the reliability and accuracy of this flow-based method. This is the first time this family of herbicides has been simultaneously analyzed by on-line SPE-MSC using a monolithic column.