Octyl‐modified magnetic graphene as a sorbent for the extraction and simultaneous determination of fragrance allergens, musks, and phthalates in aqueous samples by gas chromatography with mass spectrometry

• Published in: Journal of separation science 2015-11, Vol.38 (21), p.3758-3765
• Main Authors: Maidatsi, Katerina V, Chatzimitakos, Theodoros G, Sakkas, Vassilios A, Stalikas, Constantine D
• Format: Article
• Language: English
• Subjects: Adsorption; Allergens; Allergens - analysis; amines; Analytical chemistry; biological treatment; Chromatography; Extraction; Fatty Acids, Monounsaturated - analysis; Fragrances; gas chromatography-mass spectrometry; Gas Chromatography-Mass Spectrometry - methods; GC-MS; Graphene; Graphite - chemistry; hydrophobicity; lakes; Magnetic octyl-graphene; Magnetics; Mass spectrometry; Musk; Musks; Nanoparticles; odors; Osmolar Concentration; Perfume - chemistry; Phthalates; Phthalic Acids - analysis; Plants (organisms); Solid Phase Extraction; Sorbents; Water Pollutants, Chemical - analysis
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201500578

An effective, simple, and low‐cost sample preparation method based on dispersive SPE followed by GC with MS is developed for the multianalyte determination of fragrance allergens, musks, and phthalates, at sub‐ppb levels. The extraction procedure is based on a novel magnetic graphene sorbent, which is functionalized with octylamine, taking advantage of the functionalization's hydrophobic properties and π–π interactions with the analytes. Two alkyl amines, the octylamine and octadecylamine are studied to introduce alkyl chains in the basal plane of graphene. Magnetic graphene‐ octadecylamine is proved to be highly hydrophobic to such a degree that is hard to disperse in the bulk aqueous matrixes. Because of this behavior, its extraction efficiency for the target analytes is low. The synthesis and applicability of the magnetic graphene‐octylamine as more favored sorbent are optimized in terms of the most determining experimental conditions. The detection and quantification limits, which are calculated based on S/N ratio of 3 and 10, respectively, ranged from 0.29 to 3.2 ng L⁻¹ and from 0.89 to 9.6, respectively. The dispersive SPE is successfully applied to routine analysis for the determination of the target analytes in samples from municipal treatment plant of Ioannina (Greece), from Pamvotis Lake and baby bathwater. The reproducibility of the spiked biological treatment plant water sample is evaluated and the relative standard deviation values range between 2.1 and 9.4%.