Validation of a gas chromatography-mass spectrometry method for the determination of pg/ml levels of 17beta-estradiol and 17beta-trenbolone in bovine serum.
A method for the quantitation of pg/ml levels of 17beta-estradiol and 17beta-trenbolone in bovine serum by gas chromatography/electron-capture mass spectrometry has been developed and validated. Using the area ratios of the integrated molecular-ion peaks of the analytes to their corresponding deuterated internal standards, [2,4,16,16-2H4] 17beta-estradiol (17beta-estradiol-d(4)) and [16,16-2H2] 17beta-trenbolone (17beta-trenbolone-d(2)), and non-weighted linear regression, two calibration curves per analyte; 5-50 and 50-500 pg/ml for 17beta-estradiol in sera, and 25-250 and 250-2500 pg/ml for 17beta-trenbolone in sera, respectively, were constructed. Splitless injection of 200 fg 17beta-estradiol and 1000 fg 17beta-trenbolone could be detected and quantified. Tested batches of control bovine sera did not exhibit interference for 17beta-trenbolone, and showed expected background presence of endogenous 17beta-estradiol. Intra-day residual errors did not exceed 20%, and regression correlations were greater than 0.99. Intra-day precision data was similar to inter-day precision data. Using this method, 16 samples can be processed within one working day.
Fedeniuk
Rick W
RW
Canadian Food Inspection Agency, Saskatoon Laboratory, Centre for Veterinary Drug Residues, 116 Veterinary Road, Saskatoon, SK, Canada, S7N 2R3. rfedeniuk@inspection.gc.ca
Boison
Joe O
JO
MacNeil
James D
JD
D000818:Animals; D002138:Calibration; D002417:Cattle; D004958:Estradiol / Q000097:blood*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014204:Trenbolone Acetate / Q000097:blood*
D004958:Estradiol; D014204:Trenbolone Acetate