Determination of drugs used in advanced breast cancer by capillary gas chromatography of pharmaceutical formulations

摘要

A capillary gas chromatographic method with flame ionisation detection (FID) has been developed for the analysis of Tamoxifen, Anastrozole, and Letrozole in their pharmaceutical preparations, using Clomipramine as the internal standard in order to achieve quantification. Optimal conditions were investigated: column head pressure (110 kPa), injector and detector (FID) temperatures (both 325 ℃), time and temperature for the splitless step (0.75 min and 70 ℃), volume injected (2 μL), and an oven temperature program providing analysis times shorter than 8 minutes. The principal aspects of the validation method are examined and discussed. A test of the ruggedness of this method was carried out using the Plackett-Burman fractional factorial model with a matrix of fifteen experiments. Detection limits of 17.0, 9.6, and 30.6 μg L~(-1) were obtained for Tamoxifen, Anastrozole, and Letrozole, respectively. This method is simple, rapid, and sensitive; it was tested on the analysis of pharmacetical preparations, achieving recoveries between 98.8% and 100.3%.