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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

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Abstract: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 I -L 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 NIST mass spectral library. A I -L sample usually provides insufficient analyte for full scan data acquisition. This paper describes an on-site extraction method developed at the U.S. Environmental Protection Agency (USEPA)- Las Vegas Nevada - 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 swnple extraction, the light-
weight cartridges are easily transported and stored.



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Citation:Osemwengie, L. I., and S. Steinberg. 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. JOURNAL OF CHROMATOGRAPHY 932(1-2):107-118, (2001).
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Contact: Chris Siebert - (702) 798-2234 or siebert.christopher@epa.gov
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Division: Environmental Sciences Division
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Branch: Environmental Chemistry Branch
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Product Type: Journal
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Published: 09/30/2001
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Related Entries:
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Bullet Item Addressing Emerging Issues in Water Quality Through Environmental Chemistry
spacer Relationship Reason:   A Project of the Product
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Last Updated on Monday, October 22, 2007
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