A hybrid material as a sorbent phase for the disposable pipette extraction technique enhances efficiency in the determination of phenolic endocrine-disrupting compounds

• Published in: Journal of Chromatography A Vol. 1513; pp. 42 - 50
• Main Authors: Corazza, Gabriela, Merib, Josias, Magosso, Hérica A., Bittencourt, Otávio R., Carasek, Eduardo
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01-09-2017
• Subjects: Adsorption; Chromatography, High Pressure Liquid; DPX; Endocrine Disruptors - analysis; Hydrogen-Ion Concentration; Limit of Detection; Microscopy, Electron, Scanning; Phenol - analysis; Phenolic compounds; Pyridinium Compounds - chemical synthesis; Sample preparation; Sensitivity and Specificity; Siloxanes - chemical synthesis; Solid Phase Extraction; Sorbent phase; Spectroscopy, Fourier Transform Infrared; Surface Properties; Water Pollutants, Chemical - analysis; Sorbent phase; Sample preparation; Phenolic compounds; DPX
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2017.07.050

•A hybrid material is proposed as a new sorbent phase for the DPX technique.•Phenolic endocrine disruptor compounds were determined using the new sorbent.•The extraction efficiency was compared to a commercial DPX/styrene-divinylbenzene.•The stability of the sorbent material in organic solvents was evaluated.•Chemical interactions of the new sorbent coating with the analytes are exploited.
In this study, the hybrid material 3-n-propyl(3-methylpyridinium) silsesquioxane chloride (Si3Py+Cl−) was synthesized and investigated as a novel sorbent phase for the disposable pipette extraction (DPX) technique coupled to high-performance liquid chromatography-florescence detection. This sorbent phase was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Aqueous samples containing the phenolic endocrine-disrupting compounds bisphenol A (BPA), 17α-ethynylestradiol (EE2), 4-tert-octylphenol (4-t-OP), 4-octylphenol (4-OP) and 4-nonylphenol (4-NP) were subjected to DPX procedures and a series of optimizations was performed to determine the ideal extraction conditions using this approach. The proposed sorbent phase exhibited higher extraction efficiency than DPX-RP (reversed phase tips containing styrene-divinylbenzene), commonly used for the determination of the phenolic endocrine- disrupting-compounds under study. Satisfactory analytical performance was achieved with linear ranges from 2 to 100μgL−1 for 4-t-OP and 1–100μgL−1 for the other analytes. Limits of detection of 0.60μgL−1 for 4-t-OP and 0.30μgL−1 for other analytes, RSDs ranging from 1 to 20% and relative recoveries of 83–116% were obtained. Based on these satisfactory results, this sorbent phase represents a valuable alternative for the extraction of compounds with polar moieties in their structure.