A sensitive and specific GLC method for the determination of urinary chlorthalidone levels was developed using on-column methylation. Chlorthalidone is converted to a tetramethylated derivative with trimethylanilinium hydroxide in methanol. This method which permits the determination of as little as 0.1 microgram of chlorthalidone/ml of dog urine, should be adequate for use with human subjects receiving a clinical dose.

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