Triclosan

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Triclosan

• One Example of How Emerging Pollutants Come to
  Our Attention
• Steven Reimer
• EPA Region 10 Laboratory

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1997 1998 Region 10 Laboratory

• CRITFC Project 300 fish samples for broad
  spectrum of organics and metals
• First large scale survey of fish for consumption
  in area
• Lab participated in identifying target list
• Found usual suspects

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PCB Aroclor Analysis

• Extra peaks on ECD eluting after Aroclor 1260
• Present in bottom dwelling and older fish
• Did not match Aroclor 1268 or chlorinated
  terphenyl pattern
• Analysis on GC with Atomic Emission Detector
  showed bromine, not chlorine!

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Mystery Bromine Compounds

• Identified Brominated Diphenyl Ethers as probable
• No commercially available standard so homemade
  Bromkal 70 generated to make a standard
• Able to report total PBDE from this analysis

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2001 - 2002

• Standards available through Cambridge Isotopes
• Revisit same fish samples, this time with
  individual standards
• Check homemade standard vs storebought
• Look for sources in environment

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Potential Sources, based on Literature

• WWTP effluent water and sludge
• Storm water runoff
• Industrial effluent

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Sampling of Possible Sources

• Five WWTP from Industrial (Tacoma) to
  agricultural (Yakima) to residential (Port
  Orchard)
• Sediments above and below the outfalls for each
  WWTP
• Biosolids end user

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Procedure

• Soxhlet Extraction
• Florisil treatment
• Acid treatment
• Sulfur removal
• GC/ECD analysis

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Frustration!
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Maybe it isnt sulfur

• GC / Mass Spectrometer
• Clearly a chlorophenol 5-chloro-2-(2,4-dichloroph
  enoxy)phenol
• Need a quick standard for comparison
• Toothpaste (Colgate) extract used 0.3 triclosan
• Standard ordered from Aldrich

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What was there?
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Why did this work?

• Time to work on extras
• Equipment, especially AED and MS to ID unknowns
• Able to find standards. PBDE standards were not
  available in 97
• Picky analysts
• Luck!

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Credit where credit is due

• Bob Rieck analysis, sample prep and cleanup,
  project direction
• Randy Cummings analysis, deity of AED and user
  of Colgate
• Dave Terpening, Doc Thompson, and Jed Januch
  sampling under trying circumstances