On-site solid-phase extraction and laboratory analysis of ultra-trace synthetic musks in municipal sewage effluent using gas chromatography-mass spectrometry in the full-scan mode

Fragrance materials such as synthetic musks in aqueous samples, are normall y determined by gas chromatography-mass spectrometry in the selected ion mo nitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extr action of 1-1 samples. Full-scan mass spectra are required to verify that a target analyte has been found by comparison with the mass spectra of fragr ance compounds in the National Institute of Standards and Technology (NIST) mass spectral library. A 1-1 sample usually provides insufficient analyte for full scan data acquisition. This paper describes an on-site extraction method developed at the US Environmental Protection Agency (Las Vegas, NV, USA) for synthetic musks from 60 l of wastewater effluent. Such a large sam ple volume permits high-quality, full-scan mass spectra to be obtained for a wide array of synthetic musks. Quantification of these compounds was achi eved from the full-scan data directly, without the need to acquire SIM data . The detection limits obtained with this method are an order of magnitude lower than those obtained from liquid-liquid and other solid-phase extracti on methods. This method is highly reproducible, and recoveries ranged from 80 to 97% in spiked sewage treatment plant effluent. The high rate of sorbe nt-sample mass transfer eliminated the need for a methanolic activation ste p, which reduced extraction time, labor, and solvent use. More samples coul d be extracted in the field at lower cost. After sample extraction, the lig ht-mass cartridges are easily transported and stored. Published by Elsevier Science.