title: Determination of sulfamethazine in swine and cattle feed by reversed-phase liquid chromatography with post-column derivatization: collaborative study.
abstract: A liquid chromatographic (LC) method for the analysis of sulfamethazine (SMT) in complete swine and cattle feed was collaboratively studied. The method uses post-column derivatization with dimethylaminobenzaldehyde and detection at 450 nm. To 5g finely ground feed, extractant (0.2N HCl + 1.5% diethylamine in 25% methanol), and internal standard solutions are added, and the SMT is extracted by shaking for 1 h. Clarified extract (high-level sample extract diluted to a target concentration of ca 5.5 microg/mL) is chromatographed on a Cla reversed-phase LC column with acetonitrile-2% acetic acid (17 + 83) mobile phase. Sulfamerazine is used as an internal, or surrogate standard to correct for variable recovery of sulfamethazine from a variety of feed matrixes. Six Youden matched-pair samples were sent to 10 collaborators in Korea, Canada, and the United States. Label claims on the commercial feeds ranged from 0.0077 to 0.22% SMT. The SMT mean recovery as determined from the 5 samples with known analyte content was 99.8%. The within-laboratory relative standard deviation (repeatability) ranged from 0.28 to 4.72%. Among-laboratory (including within-laboratory) relative standard deviation (reproducibility) ranged from 1.26 to 4.87%. The authors recommend the method for AOAC INTERNATIONAL Official First Action status.
authors.affiliation: Office of Indiana State Chemist, Purdue University, West Lafayette 47907-1154, USA.
authors.forename: R L
authors.initials: RL
authors.lastname: Smallidge
authors.forename: K
authors.initials: K
authors.lastname: Albert
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D000890:Anti-Infective Agents / Q000032:analysis*; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000706:statistics & numerical data; D007202:Indicators and Reagents; D007753:Laboratories; D011786:Quality Control; D015203:Reproducibility of Results; D013418:Sulfamethazine / Q000032:analysis*; D013552:Swine
chemical_list: D000890:Anti-Infective Agents; D007202:Indicators and Reagents; D013418:Sulfamethazine