Gas Chromatographic Determination of Glucocorticoids as Trimethylsilyl Ether Derivatives

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Abstract
Glucocorticoids, e.g., dexamethasone (DM), fluocinolone acetonide (FA), triamcinolone acetonide (TA), cortisone (CS) and corticosterone (CST), were determined by gas chromatography including trimethylsilylation. In method A, a solution of 5-50 .mu.g of each glucocorticoid and 5 .mu.g of cholesterol as an internal standard dissolved in 0.2 ml of N,0-bis(trimethylsilyl)acetamide (BSA) or N,0-bis(trimethylsilyl)trifluoroacetamide (BSTFA) containing 5 mg of sodium acetate was heated at 60-80.degree. for 2-3 h. Two .mu.l of the solution was analyzed by gas chromatography. In method B, 20 .mu.l of the solution obtained in method A was transferred to a sample tube, evaporated under a stream of N, and the residue dissolved in 40 .mu.l of carbon tetrachloride, 2 .mu.l of which was analyzed by gas chromatography. FA was determined by method A, and DM, TA, CST and CS by method B. Method B was applied to commercial DM tablets, and the results were compared with those obtained by UV and BT [blue tetrazolium] methods. The values by method B were lower than those by UV method, and were almost the same as those by BT method. The trimethylsilyl derivative of DM was proved to be a tetratrimethylsilyl compound by gas chromatography-mass spectroscopy.

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