Antimony (Sb) is a nonessential metal to life and is currently considered an emerging contaminant due to its increasing presence in the environment and its toxic effects on humans, plants, and animals. Human activities such as mining, smelting, and burning of fossil fuels, along with the minerals erosion and waste, release antimony into soil and water, posing a serious threat to ecosystems and public health. The objective of this study was to evaluate trace levels of Sb(III) in water samples from the northern and central regions of Argentina using a novel methodology. Sb(III) was complexed with the fluorophore 1,4-dihydroxy-9,10-anthraquinone (quinizarin, QZ) followed by solid-phase extraction using filter paper pretreated with hexadecyltrimethylammonium bromide (HTAB). The analyte was subsequently quantified by solid surface fluorescence (λem = 575, λexc = 490). At optimal experimental conditions, the calibration curve was linear from 2.69 to 4.6 × 105 ng∙L−1 of Sb(III) (R2 = 0.9983) with a detection limit of 1.22 ng∙L−1 and a quantification limit of 2.69 μg∙L−1. Samples of mains, natural and bottled (untreated) water from 10 Argentine provinces were successfully analyzed, with an average recovery close to 100%. Solid-phase extraction demonstrated efficacy in removing potential interfering ions. Reproducibility (inter-day precision) was evaluated over 5 days, performing five daily determinations, and the CV obtained was 0.37. The results were validated using electrothermal atomic absorption spectrometry (ETAAS) with good agreement. The new methodology has a low operating cost, is easy to implement, and does not require organic solvents. The sensitivity and selectivity achieved through solid-phase extraction make it a suitable alternative to conventional techniques for determining traces of Sb(III).
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