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Determination of residual clopidol in chicken muscle by capillary gas chromatography/mass spectrometry.

Journal of AOAC International (2005-09-13)
Limin He, Yahong Liu, Zhenling Zeng, Xianhui Huang, Rong Liu
ABSTRACT

Clopidol was extracted from chicken with acetonitrile, and the extract was evaporated to about 5 mL. The concentrated solution was centrifuged and applied to a glass column filled with basic alumina. The column was eluted with methanol and the methanol was evaporated to dryness. The residue was derivatized with Sylon BFT and analyzed by gas chromatography/mass spectrometry (GC/MS). Mass characteristics of trimethylsilyl derivative of clopidol were interpreted manually. The selected-ion monitoring mode was performed at m/z 191, 248, 263, and 265. A sensitive, reproducible GC/MS method was developed for monitoring residues of clopidol in chickens. All recoveries of the drug from chicken muscle fortified at 1, 10, and 100 ng/g were > 65%, and relative standard deviations were < 15%. The detection limit was about 0.5 ng/g, and the quantitation limit was the lower limit of the standard curve, which was about 1 ng/g.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Trimethylsilanol, ≥97.5% (GC)
Sigma-Aldrich
Potassium trimethylsilanolate, 90%, technical grade
Sigma-Aldrich
Tris(trimethylsilyl) phosphite, ≥95.0% (GC)
Sigma-Aldrich
Sodium trimethylsilanolate, 95%
Sigma-Aldrich
Lithium trimethylsilanolate, 95%
Supelco
Clopidol, VETRANAL®, analytical standard

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