methimazole and pentafluorobenzyl-bromide

A method for determination of thyreostatic residues in animal tissues by matrix solid-phase dispersion (MSPD) and gas chromatography-mass spectrometry in selected ion detection mode was developed. Thyreostatic compounds in different matrices were extracted and purified by combination of MSPD and subsequent solid-phase extraction. Silica gel was selected as the solid support of both procedures and the conditions of the procedures were optimized. Thyreostats were derivatized with pentafluorobenzylbromide (PFBBr) in strong basic medium and then with N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA), which can improve the yields of derivatization for thyreostats, the repeatability, and therefore the limits of detection (LOD) of thyreostats. The limits of detection reached 10 microg/kg (2-thiouracil, 6-methyl-2-thiouracil and 6-propyl-2-thiouracil), 20 microg/kg (6-phenyl-2-thiouracil) and 50 microg/kg (tapazole) with high recoveries (more than 70% for most of thyreostats) and relative standard deviations between 4.5% and 8.7%.

Topics: Acetamides; Animals; Antithyroid Agents; Fluoroacetates; Fluorobenzenes; Gas Chromatography-Mass Spectrometry; Methimazole; Methylthiouracil; Propylthiouracil; Reproducibility of Results; Sensitivity and Specificity; Silica Gel; Silicon Dioxide; Swine; Thiouracil; Trimethylsilyl Compounds

A gas chromatography--mass spectrometry method for quantitation of the thyreostatic agent methimazole in plasma is described. The drug was transferred from the plasma sample and derivatized in one step by extractive alkylation. Either of two alkylating agents benzyl-chloride or pentafluorobenzyl bromide were used. Deuterium-labelled methimazole was used as internal standard. The precision of the method at the level of 5 ng methimazole per ml plasma was 6%.

Topics: Alkylation; Benzyl Compounds; Fluorobenzenes; Gas Chromatography-Mass Spectrometry; Humans; Methimazole