Determination of the hormonal growth promoter 17alpha-methyltestosterone in food-producing animals: bovine hair analysis by HPLC-MS/MS.
This paper describes the development, validation and application of a confirmatory method to detect 17alpha-methyltestosterone (MT) in bovine hair, to aid in controlling the administration of this growth promoter in meat-producing animals. After cryogenic grinding, MT was removed from the hair matrix using a single step extraction procedure with acetonitrile. Hydroxylamine derivatisation was used to enhance analyte determination with an electrospray ionisation (ESI) source. Determination was carried out using a triple quadrupole liquid chromatography tandem mass spectrometer (LC-MS/MS) in multiple reaction monitoring mode (MRM). The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC and using deuterated testosterone (T-d(3)) as the internal standard. The decision limit (CCalpha) was 0.07 ng g(-1) and the detection capability (CCbeta) was 0.12 ng g(-1). Repeatability was CV% (7%), within-laboratory reproducibility was CV% (11.0%), and trueness was (87%). Applicability of the method was demonstrated in an animal study. Samples obtained from animal experiments were analyzed and the presence of MT was confirmed.
Regal
P
P
Analytical Chemistry, Nutrition and Bromatology, Veterinary Faculty, University of Santiago de Compostela, 27002-Lugo, Spain.
Nebot
C
C
Vázquez
B I
BI
Cepeda
A
A
Fente
C A
CA
D045930:Anabolic Agents / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification / Q000493:pharmacokinetics; D053000:Analytic Sample Preparation Methods; D000728:Androgens / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification / Q000493:pharmacokinetics; D000818:Animals; D002138:Calibration; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification / Q000493:pharmacokinetics; D005506:Food Contamination / Q000517:prevention & control; D006197:Hair / Q000737:chemistry*; D019811:Hydroxylamine / Q000737:chemistry; D057230:Limit of Detection; D008777:Methyltestosterone / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification / Q000493:pharmacokinetics; D010858:Pigmentation; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry
D045930:Anabolic Agents; D000728:Androgens; D019811:Hydroxylamine; D008777:Methyltestosterone