title: Expansion of the Scope of AOAC First Action Method 2012.25--Single-Laboratory Validation of Triphenylmethane Dye and Leuco Metabolite Analysis in Shrimp, Tilapia, Catfish, and Salmon by LC-MS/MS.
abstract: Prior to conducting a collaborative study of AOAC First Action 2012.25 LC-MS/MS analytical method for the determination of residues of three triphenylmethane dyes (malachite green, crystal violet, and brilliant green) and their metabolites (leucomalachite green and leucocrystal violet) in seafood, a single-laboratory validation of method 2012.25 was performed to expand the scope of the method to other seafood matrixes including salmon, catfish, tilapia, and shrimp. The validation included the analysis of fortified and incurred residues over multiple weeks to assess analyte stability in matrix at -80°C, a comparison of calibration methods over the range 0.25 to 4 μg/kg, study of matrix effects for analyte quantification, and qualitative identification of targeted analytes. Method accuracy ranged from 88 to 112% with 13% RSD or less for samples fortified at 0.5, 1.0, and 2.0 μg/kg. Analyte identification and determination limits were determined by procedures recommended both by the U. S. Food and Drug Administration and the European Commission. Method detection limits and decision limits ranged from 0.05 to 0.24 μg/kg and 0.08 to 0.54 μg/kg, respectively. AOAC First Action Method 2012.25 with an extracted matrix calibration curve and internal standard correction is suitable for the determination of triphenylmethane dyes and leuco metabolites in salmon, catfish, tilapia, and shrimp by LC-MS/MS at a residue determination level of 0.5 μg/kg or below.
authors.affiliation: U.S. Food and Drug Administration, Office of Regulatory Affairs, Animal Drugs Research Center, Denver Federal Center Bldg 20, W. 6th Ave and Kipling St, Denver, CO 80225, USA.
authors.forename: Wendy C
authors.initials: WC
authors.lastname: Andersen
authors.forename: Christine R
authors.initials: CR
authors.lastname: Casey
authors.forename: Marilyn J
authors.initials: MJ
authors.lastname: Schneider
authors.forename: Sherri B
authors.initials: SB
authors.lastname: Turnipseed
mesh_terms: D000818:Animals; D002138:Calibration; D002397:Catfishes; D002851:Chromatography, High Pressure Liquid; D004396:Coloring Agents / Q000032:analysis*; D004350:Drug Residues; D005840:Gentian Violet; D057230:Limit of Detection; D033561:Penaeidae; D015203:Reproducibility of Results; D012394:Rosaniline Dyes; D012474:Salmon; D017747:Seafood / Q000032:analysis*; D053719:Tandem Mass Spectrometry; D017210:Tilapia; D014320:Triphenylmethyl Compounds / Q000032:analysis* / Q000493:pharmacokinetics
chemical_list: D004396:Coloring Agents; D012394:Rosaniline Dyes; D014320:Triphenylmethyl Compounds; C005095:malachite green; C475159:leucocrystal violet; C046945:triphenylmethane; C015320:leucomalachite green; D005840:Gentian Violet