Determination of chlorpheniramine maleate and tincture ipecac in dosage form by liquid chromatography with ultraviolet detection.

A procedure was developed and validated for measuring chlorpheniramine maleate and tincture ipecac (as emetine hydrochloride) by reversed-phase liquid chromatography with methanol-10 mM sodium heptanesulfonate (20 + 30) as the mobile phase; the pH was adjusted to 4 with acetic acid, and the flow rate was at 1.5 mL/min, with ultraviolet detection at 254 nm. Propyl paraben was used as the internal standard. The standard curves were linear (r = 0.998 and 0.9998) for both chlorpheniramine maleate and emetine hydrochloride over the ranges of 5-100 and 0.1-40 microg/mL, respectively. The mean recoveries +/- standard deviation were 101.37 +/- 2.77% for chlorpheniramine maleate and 98.8 +/- 1.47% for emetine hydrochloride. The proposed method was applied to the determination of chlorpheniramine maleate alone in tablet and syrup dosage forms. The method also was applied to the determination of the emetine content of ipecac liquid extract and tincture ipecac; the results were compared with those of the method of the British Pharmacopoeia. The proposed method was applied successfully to the simultaneous determination of chlorpheniramine maleate and tincture ipecac, as emetine hydrochloride, in syrup dosage form. Both drugs and the internal standard were separated from all interfering components in < 5 min. The proposed method is simple, specific, and economical, when compared with other published methods that determine each component alone.

Liquid chromatographic determination of fluoxetine.

A simple, accurate and sensitive high pressure liquid chromatographic technique is described for the determination of fluoxetine in the capsule dosage form, human plasma and in biological fluid. Analysis is performed with a reversed phase-C18 column with ultraviolet detection at 228 nm. The isocratic mobile phase (1.5 ml/min.) consists of acetonitrile and triethylamine buffer (48 + 52, V/V). A linear calibration model (correlation coefficient 0.99863) was developed using pyridoxine as internal standard. The retention times were 2.10 and 3.20 min for pyridoxine and fluoxetine, respectively. The method was applied for the quantitation of fluoxetine in spiked human plasma samples. The detection limit is 5 microg/l and the absorbance varies with fluoxetine concentrations in the range (10-300) microg/l. The mean % recovery +/- S.D. was found to be 97.99% +/- 2.39. The proposed method was applied successfully for monitoring of fluoxetine in human plasma after single dose administration of one prozac capsule.