Carrageenan-functionalized mesoporous silica for preconcentration and determination of 1,4-dioxane in surfactants, washing and cosmetic products by gas chromatography

• Published in: Microchemical journal 2024-12, Vol.207, p.112153, Article 112153
• Main Authors: Fedorchuk, Olga, Usov, Denys, Kobylinska, Natalia
• Format: Article
• Language: English
• Subjects: Gas chromatography coupled to tandem mass spectrometry (GC–MS/MS); Gas chromatography with flame ionization detection (GC/FID); Headspace analysis; Residual 1,4-dioxane; Sodium lauryl ether sulfate; Solid phase extraction
• ISSN: 0026-265X
• DOI: 10.1016/j.microc.2024.112153

[Display omitted] •A HS-SPE-GC/FID procedure was developed for extraction of 1,4-dioxane from surfactants, washing and cosmetic products.•Novel polysaccharide-functionalized mesostructured silica was synthesised via layer-by-layer chemical assembly method.•The developed method showed linearity in the range from 0.5 μg/L to 10.0 mg/L and the highest LOQ at 1.83 μg/L.•The developed HS-SPE-GC/FID procedure was fully validated according to ICH/Q2/R2 guideline.•GC–MS/MS with EI technique was used as arbitration method to determine 1,4-dioxane in real products. A sensitive and available static headspace-solid phase extraction method followed by gas chromatography–flame ionization detection (HS-SPE-GC/FID) was developed for the preconcentration and determination of 1,4-dioxane from raw materials and resulted products. The new λ-carrageenan-functionalized mesostructured silica (SBANH2Car) was evaluated as adsorbent for HS-SPE-GC/FID procedure. The obtained adsorbent shows mesoporous architecture with developed porosity and ordered SBA-15 type structure. The involved adsorption mechanism might be through normal phase/strong cation-exchange binding of protonated amino groups to organic functional groups such as hydroxyl, carboxyl, amino and sulfonic groups. Introduction of polysaccharide fragments onto the mesoporous silica surface and their thermal stability up to 200 °C were confirmed by the TGA analysis. The optimization of main factors which may influence on the analytical performance of the developed method, including weight of sorbents and volume of the samples used in both steps. Also, evaporation and extraction temperature and time were evaluated. The developed method provides an excellent preconcentration ability for 1,4-dioxane with the fast adsorption/desorption kinetics. Under the optimum extraction conditions, the developed HS-SPE-GC/FID procedure was validated according to ICH/Q2/R2 guideline. The obtained LOD values for the target analyte were 0.52 μg/L for surfactant and 0.61 μg/L for shampoo with a linear range from 0.1µg/L to 10 mg/L, respectively. A method based on static headspace-solid phase extraction and gas chromatography coupled to tandem mass spectrometry (GC–MS/MS) has been also validated as suitable arbitrage method. This method has offered excellent quality parameters for instance linearity (R2 > 0.9999), LOD (0.05 µg/L) and LOQ (0.15 µg/L) values without matrix effect. Finally, the proposed HS-SPE-GC/FID procedure was successfully appli