Rapid quantitative analysis of magnesium stearate in tablets using laser-induced breakdown spectroscopy.

PURPOSE: Laser-induced breakdown spectroscopy (LIBS) was evaluated for its potential as a process analytical tool for the rapid determination of magnesium stearate (MgSt) distribution within and between tablets as well as between batches in a typical manufacturing run, and for the comparison of direct-compression and roller-compaction processes. METHODS: These studies were conducted using a prototype instrument and a commercial PharmaLIBS unit, both based on pulsed Nd:YAG laser radiation at 1064 nm. The intensity of a magnesium spectral line either at 517.27 or 518.36 nm was used, depending on the product, to quantitate the MgSt concentration in the tablets. RESULTS: Using internal standardization, it was possible with the prototype instrument to accurately quantitate MgSt at the 0.5% level in two different products. For eight batches of one product, using 10 tablets from each batch, the intra-tablet, intra-batch, and inter-batch MgSt %RSDs were found to be 13.8%, 5.4% and 7.4%, respectively. Further studies were conducted with the commercial LIBS unit, which showed similar performance as the prototype unit. In particular, it was found that different depth-profile distributions of MgSt were associated with roller-compacted tablets and direct-compressed tablets. CONCLUSION: These findings illustrate the potential of LIBS to be developed as a process analytics tool for the direct and rapid determination of MgSt content and distribution in tablets.

Rapid analysis of liquid formulations containing sodium chloride using laser-induced breakdown spectroscopy.

The purpose of this work was to demonstrate the possibilities offered by laser-induced breakdown spectroscopy (LIBS) for the direct and rapid analysis of pharmaceutical liquid formulations. Sodium chloride in solution was chosen as a model compound. A pulsed Nd:YAG laser (1064 nm) was used to produce a gaseous plasma from the liquid sample. The ensuing plasma emission was spectrally analysed, and the intensity of an atomic line from sodium was used to quantitate the sodium chloride. Using surface analysis of a flowing solution, the precision (%R.S.D.) of a measurement lasting 50 s (average of 50 laser shots at 1 shot/s) was approximately 0.5% for isotonic solutions. On a non-flowing solution, a 50 s measurement had an R.S.D. of 1.8%. Direct analysis in closed (transparent) bottles was possible but more complex, requiring the superimposition of two sequential laser sparks. Using a surface procedure, common commercial isotonic products (including injectable, bacteriostatic injectable, and nasal solutions) were analysed. Their sodium content (corresponding to 0.9% sodium chloride) was accurately determined in all cases, demonstrating the capabilities of LIBS for the rapid analysis of liquid pharmaceutical products.

Influence of Er:YAG and Nd:YAG wavelengths on laser-induced breakdown spectroscopy measurements under air or helium atmosphere.

Laser-induced breakdown spectroscopy (LIBS) is widely dependent on the conditions of its implementation in terms of laser characteristics (wavelength, energy, and pulse duration), focusing conditions, and surrounding gas. In this study two wavelengths, 1.06 and 2.94 microm, obtained with Nd:YAG and Er:YAG lasers, respectively, were used for LIBS analysis of aluminum alloy samples in two conditions of surrounding gas. The influence of the laser wavelength on the laser-produced plasma was studied for the same irradiance by use of air or helium as a buffer gas at atmospheric pressure. We used measurements of light emission to determine the temporally resolved space-averaged electron density and plasma temperature in the laser-induced plasma. We also examined the effect of laser wavelength in two different ambient conditions in terms of spectrochemical analysis by LIBS. The results indicate that the effect of the surrounding gas depends on the laser wavelength and the use of an Er:YAG laser could increase linearity by limiting the leveling in the calibration curve for some elements in aluminum alloys. There is also a significant difference between the plasma induced by the two lasers in terms of electron density and plasma temperature.