A novel approach for simultaneous determination of 2‐mercaptobenzimidazole and derivatives of 2‐thiouracil in animal tissue by gas chromatography/mass spectrometry

Abstract

A novel approach for determination of 2-mercaptobenzimidazole (MBI) and other thyreostatic residues in animal tissues by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode was developed. The analytes in animal tissues (including hypothyroid, pork muscle and beef samples) were extracted by acetonitrile, and then purified by a matrix solid-phase dispersion (MSPD) procedure after the extraction residues had been dissolved in water. The thyreostatic residues were derivatized by pentafluorobenzyl bromide (PFBBr) under strong basic conditions and then N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) before GC/MS analysis. Different kinds of solid supports with various polarities for the MSPD procedure were investigated, and it was found that silica gel was suitable for the purpose. The average recoveries of the thyreostatic drugs in animal tissues ranged from 71.5-96.9% with the relative standard deviations below 10%. By using the developed method, the limits of detection were 10 microg/kg for MBI; 5 microg/kg for 6-phenyl-2-thiouracil; and 2 microg/kg for 2-thiouracil, 6-methyl-2-thiouracil and 6-propyl-2-thiouracil. The stability of the thyreostatic drugs in spiked animal tissues was tested, and the results showed that the thyreostatic drugs did not decompose within 3 months if the sample was stored in darkness below -20 degrees C.