Comparison of the determination of a low-concentration active ingredient in pharmaceutical tablets by backscatter and transmission Raman spectrometry.

A total of 383 tablets of a pharmaceutical product were analyzed by backscatter and transmission Raman spectrometry to determine the concentration of an active pharmaceutical ingredient (API), chlorpheniramine maleate, at the 2% m/m (4 mg) level. As the exact composition of the tablets was unknown, external calibration samples were prepared from chlorpheniramine maleate and microcrystalline cellulose (Avicel) of different particle size. The API peak at 1594 cm(-1) in the second derivative Raman spectra was used to generate linear calibration models.

Effect of particle properties of powders on the generation and transmission of Raman scattering.

Transmission Raman measurements of a 1 mm thick sulfur-containing disk were made at different positions as it was moved through 4 mm of aspirin (150-212 μm) or microcrystalline cellulose (Avicel) of different size ranges (<38, 53-106, and 150-212 μm). The transmission Raman intensity of the sulfur interlayer at 218 cm(-1) was lower when the disk was placed at the top or bottom of the powder bed, compared to positions within the bed and the difference between the sulfur intensity at the outer and inner positions increased with Avicel particle size. Also, the positional intensity difference was smaller for needle-shaped aspirin than for granular Avicel of the same size.