Abstract
A fully automated method has been developed for the determination of eight macrocyclic musk fragrances in urban wastewater. The procedure includes the enrichment of the analytes by microextraction by packed sorbent (MEPS) followed by large volume injection–gas chromatography–mass spectrometry (LVI–GC–MS). The main factors in the MEPS technique were optimized. For all of the analytes, the highest enrichment factors were achieved when 4mL samples were extracted by using C18 MEPS-sorbent and 50μL of ethyl acetate were used for desorption. The eluate was directly analysed by GC–MS. Detection limits were found to be between 5ngL−1 and 10ngL−1, depending on the target analytes. In addition, under optimized conditions, the method gave good levels of intra-day and inter-day repeatability in wastewater samples with relative standard deviation (RSD) (n=3, 1000ngL−1) less than 5% and 9%, respectively. The applicability of the method was tested with wastewater samples from two influent and effluent urban wastewater treatment plants (WWTPs). The analysis of influent urban wastewater revealed the presence of most of the macrocylic musks at concentrations higher than the method quantification limits (MQLs), being the most abundant analyte ambrettolide at 9.29μgL−1. In addition, the analyses of effluent urban wastewater showed a decrease in the concentrations with macrocyclic musk concentrations of between not detected (n.d.) and 2.26μgL−1 being detected.
Published Version
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