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Gas Chromatographic Determination of Residues of Thyreostatic Drugs in Bovine Muscle Tissue Using Combined Resin Mediated Methylation and Extraction

Gas Chromatographic Determination of Residues of Thyreostatic Drugs in Bovine Muscle Tissue Using Combined Resin Mediated Methylation and Extraction

G Y Yu, E J Murby, R J Wells

J Chromatogr B Biomed Sci Appl. 1997 Dec 5;703(1-2):159-66.

PMID: 9448072

Abstract:

A method is described for the assay of residues of the thyreostatic substances 2-thiouracil, 6-methyl-2-thiouracil, 5- and 6-propyl-2-thiouracils and 6-phenyl-2-thiouracil in beef muscle at levels of quantitation down to 25 microg/kg for thiouracil and 15 microg/kg for substituted thiouracils. Analytes are extracted from the muscle matrix with acetonitrile and methylated by absorption onto a macroporous anion exchange resin followed by treatment with methyl iodide in acetonitrile at room temperature. Supercritical carbon dioxide is also a suitable derivatization solvent. Determination is carried out using gas chromatography with mass spectrometric detection. The methyl ester of 2,4,5-trichlorophenoxyacetic acid serves as an internal standard while 5-methyl-2-thiouracil is a suitable surrogate. 5-Ethyl-2-thiouracil is added to minimise losses of the analytes during the analysis. The method exhibits a linear range of 25-625 microg/kg for the substituted thiouracils and 50-1250 microg/kg for 2-thiouracil. Recovery of the analytes ranges from 50% for 6-phenyl-2-thiouracil to 90% for 2-thiouracil with coefficients of variation of less than 10%.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP1928376	2,4,5-T methyl ester		1928-37-6	Price

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