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Development of Analytical Methods for the Identification of Synthetic Musk Compounds in Environmental Samples

Project Purpose:
Identification of Synthetic Musk Compounds in water (trace levels), soil, biosolids, and fish tissues.

Project Description(s):
Develop trace-level screening and analytical methods sufficiently rugged to meet the needs of research scientists. In this respect, synthetic musk compounds [Galaxolide® (HHCB), Tonalide® (AHTN), Phantolide® (AHMI), Celestolide® (ADBI), Versalide® (AETT), Cashmeran® (DPMI), and Traseaolide® (ATII) in the polycyclic group and musk ambrette (MA), and musk ketone (MK), musk xylene (MX), musk muskene (MM), and musk tibetene (MT) in the nitro musk group], which occur frequently as contaminants in the environment, were selected for developing methods that may be used for testing wastewater, sludge, and biological tissues. Since synthetic musk transformation products may be indicative of sewage contamination in freshwater sources, we also synthesized nitro musk metabolites (2-amino musk xylene, 4-amino musk xylene, and amino musk ketone) and included them in the determination of both parents and transformation products in the aquatic environment.

Project Outcomes:
Project Outcomes: 1. A solid-phase (methyl methacrylate and polystyrene divinybenzene) extraction technique and laboratory ultra-trace analytical method for the determination of synthetic musk compounds "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" was develop and applied to environmental samples in the Las Vegas local ecological sites. 2. Levels of synthetic musk compounds were determined in municipal sewage effluent, Lake Mead (NV) water, and fish samples. Dr. David Epel of Hopkins Marine Station of Stanford University, Pacific Grove, CA., adopted this method and his graduate students used it to determine synthetic musk levels in the San Francisco Bay area. 3. Dr. Steven D. Mercurio and his graduate student, Mr. Eric Elias of Minnesota State University, Mankato, Department of Biological Sciences adopted this method in the determination of estrogenic compounds (tamoxifen citrate and 17-alpha-ethynylestradiol) in a hospital effluent in Minnesota. 4 Closed-loop stripping analysis of synthetic musk compounds was also developed for the screening of synthetic musks in biological tissues with sufficient adipose tissues. 5. A review of sewage sludge regulations and land application practices by the United States National Research Council in 2002, recommended development of improved analytical techniques to adequately identify and quantify new chemical contaminants, such as synthetic musk compounds in Class A sewage sludge (i.e., biosolids). Our previously developed synthetic musk compound determinative methods were applied and resulted in a rugged analytical method using gas chromatography coupled to mass spectrometry to detect this group of organic pollutants in biosolids.

Contact
Lantis Osemwengie at osemwengie.lantis@epa.gov

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