Abstract
An analytical method combining off-line solid phase extraction (SPE) and reversed phase high performance liquid chromatography (HPLC) has been developed for simultaneous determination of six herbicides. The compounds analyzed in natural surface water samples, were: the herbicides atrazine (AT), simazine (SI) and their major dealkylated and hydroxylated degradation products such as deisopropyl-atrazine (DIA), deethyl-atrazine (DEA), hydroxyl-atrazine (H-AT) and hydroxyl-simazine (H-SI), all of them with herbicide activity too. As optimum conditions, a Kromasil C18 column as stationary phase, a mixture of acetonitrile and phosphate buffer pH 7.0 as mobile phase in gradient elution mode and 215 nm as measuring wavelength, were selected. A polymeric cartridge (Bond-Elut ENV-1000 mg) was used for a SPE procedure. The optimized off-line SPE HPLC-DAD method was evaluated in terms of validation and robustness procedure, obtaining among other parameters, limits of quantification between 81 and 100 ng L-1, considering the enrichment factor for all of the studied herbicides. The proposed method was successfully applied to the screening of herbicides in natural surface water samples from different locations in the 23th aquifer (Albacete, Spain).
Highlights
Pesticides such as s-triazines are widely used as selective pre and post-emergence herbicides for the control of broadleaved, grassy areas, in many agricultural crops like corn, wheat, as well as in railways, roadside verges and golf courses
Atrazine (AT), (2chloro-N4-ethyl-N6-isopropyl-1,3,5-triazine4,6-diamine), Simazine (SI), (2chloro-N4,N6-diethyl-1,3,5-triazine4,6-diamine) and their main dealkylated and hydroxylated degradation products, Deethyl-atrazine (DEA), Deisopropyl-atrazine (DIA), hydroxyl-atrazine (H-AT) and hydroxyl-simazine (HSI), are considered inside to the group of endocrine-disrupting chemicals [1], according to U.S Environmental Protection Agency (EPA)
A sensitive, easy and simple chromatographic method has been described for the separation and quantification of endocrinedisrupting chemicals SI, AT and their major degradation products as hydroxylated and dealkylated ones, H-SI, H-AT and DIA and DEA, respectively
Summary
Pesticides such as s-triazines are widely used as selective pre and post-emergence herbicides for the control of broadleaved, grassy areas, in many agricultural crops like corn, wheat, as well as in railways, roadside verges and golf courses. The EPA defines an environmental endocrine or hormone disrupting chemical as an exogenous agent, which interferes with the synthesis, secretion, transport, binding, action or elimination of natural hormones in the body, and that are responsible for the maintenance of homeostasis, reproduction, development and/or behavior [2]. Both atrazine, simazine and their degradation products, are relatively persistent making necessary their analysis and quantification in environmental samples. Water quality receives considerable attention for its obvious implication in public health, so, stringent regulations have been issued by legislation agencies. Current European Union (EU) directives [3], dictates that concentrations of individual pesticides must not exceed maximal admissible values of 0.1 μg L-1 in drinking water, whereas in natural surface waters, the alert and alarm threshold values are typically 1 and 3 μg L-1, respectively
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