Determination of siloxanes in water samples employing graphene oxide/Fe₃O₄ nanocomposite as sorbent for magnetic solid‐phase extraction prior to GC–MS

Abstract

A new, fast, simple, and environmentally friendly analytical method has been developed to determine six siloxanes in water samples: octamethyltrisiloxane, octamethylcyclotetrasiloxane, decamethyltetrasiloxane, decamethylcyclopentasiloxane, dodecamethylpentasiloxane and dodecamethylcyclohexasiloxane. The analytical method consists of magnetic solid‐phase extraction employing graphene oxide/Fe3O4 as sorbent for the separation and preconcentration of siloxanes prior to GC–MS determination. The extraction procedure was optimized by means of a Plackett‐Burman design. Under the optimized extraction conditions (graphene oxide/Fe3O4, 20 mg; extraction time, 10 min; eluent volume, 0.5 mL ACN; elution time, 2.5 min; sample volume, 20 mL), the method rendered repeatability levels with a relative standard deviation between 9 and 20% (n = 6, 10 μg/L). Methodological limits of detection ranged from 0.003 to 0.1 μg/L. The linearity of the method was studied between the methodological limit of quantification and 100 μg/L, obtaining correlation coefficient values between 0.990 and 0.999. The applicability of the method was assessed by analyzing drinking, river and wastewater samples. Relative recovery values ranged between 70 and 120% (1 and 60 μg/L spiking level) showing that the matrix had a negligible effect on extraction. Finally, the greenness of this method was confirmed by the semiquantitative Eco‐Scale metrics.

US EPA to evaluate cyclic siloxane

“…As part of a method development study, samples of water were collected from a water purification plant (Murcia, Spain), a river water sample (Alcoy, Spain), wastewater samples from three different points of Rincón de León WWTP (three samples, WWTP1) (Alicante, Spain), from Monte Orgegia WWTP (one sample, WWTP2) (Alicante, Spain), and from a WWTP in Portugal (one sample) (Costa dos Reis et al, 2018). D4 was present in the sample from the Portuguese WWTP, at a mean concentration of 3,100 ng/L.…”

Biochar/sodium alginate mixed matrix membrane as adsorbent for in‐syringe solid‐phase extraction towards trace nitroimidazoles in water samples prior to ultra‐high‐performance liquid chromatography‐tandem mass spectrometry analysis

“…The concentration level of NDZs is low in actual samples. Several analytical methods have been reported for the determination of NDZs, including electrophoresis [4], gas chromatography (GC) [5], GC‐mass spectrometry (MS) [6], liquid chromatography (LC) [7] and LC‐MS [8]. LC‐MS is the preferred technique to analyze low levels of NDZs.…”

Enhancing Trace Metal Extraction from Wastewater: Magnetic Activated Carbon as a High-Performance Sorbent for Inductively Coupled Plasma Optical Emission Spectrometry Analysis

“…These pollutants may enter the human body through air, water, food, or absorption through the skin [6]. It is well known that exposure to certain heavy metals has been linked to a number of disorders that are harmful to human The sorbents decorated with magnetic solids simultaneously combine the exceptional sorbent capability and the easy sorbent handling, reducing analysis time, sorbent amounts, and the consumption of solvents [67,68]. Finally, analytes can be desorbed employing an eluent solvent or heating for further analysis [69].…”