Validation of a gas chromatographic method for determining fatty alcohols that compose policosanol in five-milligram film-coated tablets.

A gas chromatographic method using a packed column and 1-eicosanol as an internal standard was developed and validated for determination of the aliphatic fatty alcohols that compose policosanol in 5 mg film-coated tablets. The alcohols were analyzed as trimethylsilyl (TMS) derivatives, prepared with N-methyl-N-trimethylsilylfluoroacetamide. The method can detect degradation products with high retention times without interfering with the peaks of the active principle. Good linearity (correlation coefficient = 0.9996) and accuracy (recovery = 100.44%) were proven over a range of 50-150% of the nominal concentration. Within-day and between-day precisions at the nominal 100% value met the acceptance criteria (< 2%). Ruggedness was examined through an intralaboratory experimental study in which 7 operational changes were made and the observed results were quantitation, repeatability, resolution, and relative retention time. Among these results, only the relative retention time (tC28,C20) was significantly affected when the column used was 2.1 m instead of 3.1 m. Repeatability and reproducibility (r = 0.1506 and R = 0.2450, respectively) were obtained from a uniform-level interlaboratory test. The method is suitable for quality control and stability studies of these tablets.