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  • Improved sensitivity gas chromatography-mass spectrometry determination of parabens in waters using ionic liquids.

Improved sensitivity gas chromatography-mass spectrometry determination of parabens in waters using ionic liquids.

Talanta (2015-12-24)
Juan Ignacio Cacho, Natalia Campillo, Pilar Viñas, Manuel Hernández-Córdoba
ABSTRACT

A new procedure for the introduction of ionic liquid samples in gas chromatography (GC) is proposed. This procedure, based on microvial insert thermal desorption, allows the direct analysis of the compounds preconcentrated by ionic liquid based liquid-liquid microextraction (IL-LLME) using the combination of a thermal desorption unit (TDU) and a programmed temperature vaporization injector (PTV). Two different IL-LLME methodologies, one based on the formation of a microdroplet emulsion by dispersive liquid-liquid microextraction (DLLME) and other through ultrasound-assisted emulsification microextraction (USAEME) were studied and evaluated. IL-DLLME proved advantageous and consequently, it was adopted for preconcentration purposes. This easy to apply approach was used for the determination of five parabens (methyl-, ethyl-, propyl-, butyl- and isobutyl paraben) in swimming pool waters, after in situ acetylation. The optimized conditions of TDU/PTV allowed the analytes contained in 20 µL of the enriched IL to be transferred to the capillary column. Quantification of the samples was carried out against aqueous standards, and quantification limits of between 4.3 and 8.1 ng L(-1) were obtained, depending on the compound. Concentrations of between 9 and 47 ng L(-1) for some analytes were obtained in the analysis of ten samples.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Isobutyl 4-hydroxybenzoate, 97%
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4′-Hydroxyacetophenone, 99%
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N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, with 1% trimethylchlorosilane, for GC derivatization, LiChropur
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Butyl 4-hydroxybenzoate, SAJ first grade, ≥99.0%
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Ethyl 4-hydroxybenzoate, SAJ first grade, ≥99.0%
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Butyl 4-hydroxybenzoate, ≥99%
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N,O-Bis(trimethylsilyl)trifluoroacetamide, ≥99%
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Methyl 4-hydroxybenzoate, BioXtra, ≥99.0% (titration)
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Potassium phosphate dibasic, puriss. p.a., ACS reagent, anhydrous, ≥99.0% (T)
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Acetic anhydride, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99% (GC)
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Methyl 4-hydroxybenzoate, SAJ first grade, ≥98.0%
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Acetic anhydride, ACS reagent, ≥98.0%