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S chneider & Andersen: J ournal of AOAC International Vol. 98, No. 3, 2015 669
with responses above the 0.5 µg/kg calibrant for three or four
residues. At the 0.90 µg/kg concentration, eight analytes (2%)
generated peak areas below the response for the 0.5 extracted
matrix calibrant. Based on the single point calibrant, these
eight would yield residue concentrations in the range of 0.39
to 0.48 µg/kg. Some incurred samples were screened below the
0.5 µg/kg extracted matrix calibrant, but most of these had mean
residue concentrations below 0.4 µg/kg, making it reasonable
that these samples would be screened below the 0.5 µg/kg
matrix calibration level. One MG in shrimp “incurred” sample
yielded an estimated concentration of 0.44 µg/kg, yet the MG
incurred shrimp mean concentration was 0.71 µg/kg.
Recommendation
This method has provided clearly acceptable results at and
below the level of interest (1 µg/kg) for the triphenylmethane
dyes studied. The method accuracy was excellent with trueness
generally ≥90%, precision generally ≤10% RSDr, and HorRat
values <1. The Study Directors recommend this method for
acceptance as Final Action status.
Acknowledgments
We thank John Phillips (U.S. Department of Agriculture,
Agricultural Research Service, Wyndmoor, PA) for performing
the statistical analysis for this study.
We also acknowledge the following individuals from the
FDA for their technical assistance with the preparation of the
study samples: Sherri Turnipseed and Joseph Storey (Animal
Drugs Research Center, Office of Regulatory Affairs, Denver
Laboratory, Denver, CO); Christine Casey, Edward Iannuzzi,
Ryan Stadtmuller, Julie Lillehaugen, Andrea Heise, Zachary
Miller, Ashleigh Gillaspie, and Mark Madson (Office of
Regulatory Affairs, Denver Laboratory, Denver, CO); and
Eric Evans and Scott Frobish (Center for Veterinary Medicine
Aquaculture Program, Laurel, MD).
We thank Sherri Turnipseed and Steve Lehotay (USDA-
ARS, Wyndmoor, PA) for assistance with design of the study
protocol, Kai Klocke for assistance with programming and data
transformation, and Tom Phillips (Maryland Department of
Agriculture, Annapolis, MD) for additional statistical review.
Finally, we acknowledge the following collaborators for their
participation in this study:
Mark Crosswhite and Walter Hammack, Florida Department
of Agriculture and Consumer Services, Division of Food Safety,
Chemical Residue Laboratory, Tallahassee, FL
Christopher K. Lam and Mary Cumming, Tennessee
Department of Agriculture, Ivy Laboratory, Nashville, TN
Sarah R. Ruiz and Cheryl D. Stephenson, Eurofins Central
Analytical Laboratories, New Orleans, LA
Alan R. Lightfield and Steven J. Lehotay, U.S. Department
of Agriculture, Agricultural Research Service, Eastern Regional
Research Center, Wyndmoor, PA
Dominique Hurtaud-Pessel, Pierrick Couëdor, and Eric
Verdon, ANSES, French Agency for Food, Environmental and
Occupational Health Safety, Laboratory of Fougères, EU-RL
for Antibiotic and Dye Residues, Fougères, France
Mike Filigenzi and Robyn Noonan, California Animal Health
and Food Safety Laboratory, University of California at Davis,
Davis, CA
Anna Hawkins, Shristi Prakash, and Michael Conway, OMIC
USA Inc., Portland OR
Jason Smith and Ross Potter, Canadian Food Inspection
Agency, Dartmouth Laboratory, Dartmouth, Nova Scotia,
Canada
Robert Burger, U.S. Food and Drug Administration, Office of
Regulatory Affairs, Denver Laboratory, Denver, CO
Yanxuan Tina Cai, U.S. Food and Drug Administration,
Office of Regulatory Affairs, Northeast Regional Laboratory,
Jamaica, NY
Andrew Fong, John Kibbey, and Chris Baker, U.S. Food and
Drug Administration, Office of Regulatory Affairs, Arkansas
Regional Laboratory, Jefferson, AR
Andrew Harris and Linda Lissemore, University of Guelph,
Laboratory Services, Chemistry Unit, Guelph, Ontario, Canada
Sara Lupton, U.S. Department of Agriculture, Agricultural
Research Service Biosciences Research Laboratory, Fargo, ND
Haejung An, U.S. Food and Drug Administration, Office of
Regulatory Affairs, Pacific Regional Laboratory Southwest, Irvine,
CA
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Candidates for 2016 Method of the Year
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