Using Design of Experiments to Optimize a Screening Analytical Methodology Based on Solid-Phase Microextraction/Gas Chromatography for the Determination of Volatile Methylsiloxanes in Water

• Type: Article in International Scientific Journal
• Date: 2021

Authors

Fábio Bernardo (Author) FEUP; Providencia González-Hernández (Author) Other; Nuno Ratola (Author) FEUP; Verónica Pino (Author) Other; Arminda Alves (Author) FEUP; Vera Homem (Author) FEUP

Journal

Title: Molecules

Vol. 26 No. 11

Pages: 1-13

ISSN: 1420-3049

Publisher: MDPI

Indexing

ISI Web of Knowledge - 0 Citations

Scopus - 0 Citations

Associated Projects

AGRONAUT - Estudo do impacto agronómico da utilização de lamas de depuração através de uma perspectiva de exposição

LaNSiloT - LAunching New SILOxane Treatments: assessing effluent, sludge and air quality and improving biogas production in WWTPs

LEPABE - Financiamento Plurianual 2020-2023 da Unidade de I&D LEPABE - Laboratório de Engenharia de Processos, Ambiente, Biotecnologia e Energia

Other information

Authenticus ID: P-00V-2D8

DOI: 10.3390/molecules26113429

Abstract (EN): 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 mu m PDMS/Divinylbenzene fiber, 10 mL sample, 19.5% NaCl, 39 min extraction time, 10 min desorption time, and 33 degrees C and 240 degrees 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.

Language: English

Type (Professor's evaluation): Scientific

No. of pages: 13