Abstract
Volatile methylsiloxanes (VMSs) constitute a group of compounds used in a great variety of products, particularly personal care products. Due to their massive use, they are continually discharged into wastewater treatment plants and are increasingly being detected in wastewater and in the environment at low concentrations. The aim of this work was to develop and validate a fast and reliable methodology to screen seven VMSs in water samples, by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The influence of several factors affecting the extraction efficiency was investigated using a design of experiments approach. The main factors were selected (fiber type, sample volume, ionic strength, extraction and desorption time, extraction and desorption temperature) and optimized, employing a central composite design. The optimal conditions were: 65 µm PDMS/Divinylbenzene fiber, 10 mL sample, 19.5% NaCl, 39 min extraction time, 10 min desorption time, and 33 °C and 240 °C as extraction and desorption temperature, respectively. The methodology was successfully validated, showing low detection limits (up to 24 ng/L), good precision (relative standard deviations below 15%), and accuracy ranging from 62% to 104% in wastewater, tap, and river water samples.
Highlights
IntroductionSiloxanes are organic compounds with a backbone of alternating atoms of silicon (Si) and oxygen (O), with organic groups (e.g., methyl, ethyl, phenyl, etc.) attached to the silicon atoms [1]
Siloxanes are organic compounds with a backbone of alternating atoms of silicon (Si) and oxygen (O), with organic groups attached to the silicon atoms [1]
The aim of this study is to develop, optimize using design of experiments (DoE), and validate a solid-phase microextraction followed by gas chromatography-flame ionization detection (GC-FID) analysis for the determination of seven volatile methylsiloxanes (VMSs) (D3, D4, D5, D6, L3, L4, and L5) in aqueous samples
Summary
Siloxanes are organic compounds with a backbone of alternating atoms of silicon (Si) and oxygen (O), with organic groups (e.g., methyl, ethyl, phenyl, etc.) attached to the silicon atoms [1]. The most significant representatives are the low molecular volatile methylsiloxanes (VMSs), which are commonly incorporated in daily products such as personal care products (PCPs). Considering their chemical structure, they may be classified as linear (lVMSs) or cyclic (cVMSs) compounds [2]. Linear and cyclic methylsiloxanes are usually expressed as Ln and Dn, with “n” representing the number of silicon atoms. Due to their massive use, VMSs are continuously discharged down-the-drain, reaching wastewater treatment plants (WWTPs).
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