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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 31, Number 2, March 2007,
pp.115-118
CASE REPORT: Clenbuterol Determination in Calf Hair by
UPLC-MS–MS: Case Report of a Fraudulent Use for Cattle Growth
Guillaume Salquèbre, Marie Bresson, Marion Villain,
Vincent Cirimele, and Pascal Kintz
Laboratoire ChemTox, 3 rue Grüninger, 67400 Illkirch, France
A method for clenbuterol determination in hair has been developed.
Hair specimens collected from two calves were decontaminated using hot water
followed by methylene chloride. Hair was cut into small pieces, and 100 mg was
incubated in 1 mL 0.1M hydrochloric acid overnight at 45°C in the presence
of 1 ng acebutolol used as internal standard. After neutralization with 1 mL
0.1M NaOH, 2 mL of bicarbonate buffer (pH 8.6) were added and the preparation
was then purified using solid-phase extraction with an Isolute C18 column. Methanolic
eluent was evaporated to dryness and the residue was reconstituted with 50 µL
methanol. A 5-µL portion was injected onto an ACQUITYTM UPLC BEH C18 column
(2.1 * 50 mm, 1.7 µm) and separation was achieved using a gradient of
acetonitrile and formate buffer delivered at a flow rate of 0.6 mL/min. Detection
was done on a Waters® Micromass® Quattro Micro™ API triple-quadrupole
mass spectrometer. Ionization was achieved using electrospray in positive mode.
Clenbuterol was identified by two transitions (m/z 277.1 > 203.2 and m/z
277.1 > 132.1). Quantitation was performed with the most intensive transition
(m/z 277.1 > 203.2) versus the internal standard monitored using the transition
(m/z 337.3 > 116.1). When compared with gas chromatography methods that are
generally used for the determination of b-adrenergics, the major advantages
of this method were the sensitivity, a shorter run time, and the absence of
a derivatization step. The analysis of two hair samples from calves suspected
of drug administration showed low clenbuterol concentrations at 3.6 and 4.8
pg/mg.
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