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 normally determined by gas chromatography-mass spectrometry in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction 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 fragrance 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 sample volume permits high-quality, full-scan mass spectra to be obtained for a wide array of synthetic musks. Quantification of these compounds was achieved 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 extraction methods. This method is highly reproducible, and recoveries ranged from 80 to 97% in spiked sewage treatment plant effluent. The high rate of sorbent-sample mass transfer eliminated the need for a methanolic activation step, which reduced extraction time, labor, and solvent use. More samples could be extracted in the field at lower cost. After sample extraction, the light-mass cartridges are easily transported and stored.