Application of Near-Infrared Spectroscopy in Real-Time Monitoring of Product Attributes of Ribbed Roller Compacted Flakes

Abstract

Abstract. This study assessed the utility of near-infrared (NIR) spectroscopy for the real-time monitoring of content uniformity and critical quality attributes (tensile strength, Young's modulus, and relative density) of ribbed roller compacted flakes made by axially corrugated or ribbed rolls. A custom-built setup was used to capture off-line NIR spectra from the flakes containing micronized chlorpheniramine maleate, microcrystalline cellulose, lactose, and magnesium stearate. The partial least square regression method was employed to build calibration models from these off-line NIR spectra using experimental design and validated using test set validation. During calibration model development, various factors, such as spectral acquisition mode, probe positioning, spectral preprocessing method, and beam size, were investigated to improve the prediction ability of the models. The statistical results obtained for calibration models and their validation revealed that dynamic spectral acquisition and proper probe positioning were very crucial to minimize the incorporation of variability in NIR spectra resulting from the flake's undulation. Calibration and validation statistics also suggested the importance of selecting appropriate spectral preprocessing method and beam size. In this study, best calibration models resulted from standard normal variate followed by first derivative preprocessed dynamic spectra captured using beam sizẽ 1.2 mm. Best calibration models constructed from off-line NIR spectra were used in real-time analysis of flake attributes. Finally, adequacy of best calibration models was established from real-time prediction results. Overall, with the proposed setup, it was possible to monitor the roller compaction process in real time for various properties associated with the ribbed flakes in a rapid, efficient, and nondestructive manner.

Process analytical technology tools for process control of roller compaction in solid pharmaceuticals manufacturing

“…Most of the recent studies performed by Acevedo et al (35), Crowley et al (36), and McAuliffe et al (37), focused only on monitoring of ribbon density, demonstrating the suitability of NIR spectroscopy for evaluating ribbons of variable quality. The broad applicability of NIR spectroscopy to simultaneously determine CQAs of ribbons, such as drug content, density, tensile strength and Young's modulus of roller-compacted ribbons has also been demonstrated by Gupta et al (38), Samanta et al (39) and Quyet et al (40). Their results demonstrate the possibility of identifying overcompressed or under compressed ribbons or ribbons containing a higher or lower percentage of API in real-time.…”

Hyperspectral imaging sensor for optimization of small molecule formulations

“…The first SG derivative removes the baseline offset. However, the second SG derivative is largely preferred because it resolves nearby peaks and improves the spectral resolution in addition to removing the baseline offset (Samanta, Karande, Ng, & Heng, ). All the pre‐processing steps were conducted using the MATLAB and Unscrambler software.…”

Evaluating the Performance of Collimated Light for near Infrared Analysis of Minced Beef Samples

“…It is evident that the intensity of the signal received is higher for the fibre-optic reflectance probe than for the collimator-probe setup at a distance of 0.2 cm, which could be attributed to the reason that it is specifically designed to work at this stand-off distance. 8 However, it can be seen that the collimator-probe setup works better from a stand-off distance of 1.0 cm. Additionally, the collimator-probe setup was able to receive sufficient signal even at a stand-off distance of 5 cm, which could be attributed to the reason that light was collimated onto the 99% reflectance standard.…”