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  • Hydrophilic interaction liquid chromatography coupled to high-resolution mass spectrometry to determine artificial sweeteners in environmental waters.

Hydrophilic interaction liquid chromatography coupled to high-resolution mass spectrometry to determine artificial sweeteners in environmental waters.

Analytical and bioanalytical chemistry (2014-11-28)
Daniela Salas, Francesc Borrull, Núria Fontanals, Rosa Maria Marcé
ABSTRACT

Artificial sweeteners are food additives employed as sugar substitutes which are now considered to be emerging organic contaminants. In the present study, a method is developed for the determination of a group of artificial sweeteners in environmental waters. Considering the polar and hydrophilic character of these compounds, hydrophilic interaction liquid chromatography is proposed for their separation as an alternative to traditional reversed-phase liquid chromatography. Two stationary phases with different chemistry were compared for this purpose. For the detection of the analytes, high-resolution mass spectrometry (Orbitrap) was employed to take advantage of its benefits in terms of reliable quantification and confirmation for the measurement of accurate masses. Solid-phase extraction was chosen as the sample treatment, in which the extract in a mixture of NH4OH:MeOH:ACN (1:4:15) was directly injected into the chromatographic system, simplifying the analytical procedure. The optimized method was validated on river and waste water samples. For example, in the case of effluent water samples, limits of detection ranged from 0.002 to 0.7 μg/L and limits of quantification ranged from 0.004 to 1.5 μg/L. Apparent (whole method) recoveries ranged from 57 to 74% with intra-day precision (%RSD, n = 5) ranging from 6 to 25%. The method was successfully applied to water samples from different rivers in Catalonia and different waste water treatment plants in Tarragona. Acesulfame, cyclamate, saccharine and sucralose were found in several samples.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
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Saccharin, ≥98%
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Acetic acid, ≥99.5%, FCC, FG
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Saccharin, ≥99%
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Sodium dodecyl sulfate, ACS reagent, ≥99.0%
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Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
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Sodium dodecyl sulfate, ≥98.0% (GC)
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Sodium dodecyl sulfate, ≥90% ((Assay))
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Ammonium formate, ≥99.995% trace metals basis
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Ammonium acetate, 99.999% trace metals basis
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Methanol, anhydrous, 99.8%
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Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
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Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
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Ammonium acetate solution, for molecular biology, 7.5 M
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Ammonium acetate, for molecular biology, ≥98%
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Ammonium acetate, reagent grade, ≥98%
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Sodium dodecyl sulfate, BioXtra, ≥99.0% (GC)
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Sodium dodecyl sulfate, ReagentPlus®, ≥98.5% (GC)
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Sodium dodecyl sulfate, 92.5-100.5% based on total alkyl sulfate content basis
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Ammonium acetate, BioXtra, ≥98%
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Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology
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Sodium dodecyl sulfate, BioReagent, suitable for electrophoresis, for molecular biology, ≥98.5% (GC)
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Sodium dodecyl sulfate, tested according to NF, mixture of sodium alkyl sulfates consisting mainly of sodium dodecyl sulfate
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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
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Sodium dodecyl sulfate, BioUltra, for molecular biology, ≥99.0% (GC)
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Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
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Sodium dodecyl sulfate, ≥99.0% (GC), dust-free pellets
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