Abstract
The process analytical technology (PAT) initiative proposed by the US Food and Drug Administration (FDA) suggests innovative methods to better understand pharmaceutical processes. The development of analytical methods that quantify active pharmaceutical ingredients (APIs) in powders and tablets is fundamental to monitoring and controlling a drug product’s quality. Analytical methods based on vibrational spectroscopy do not require sample preparation and can be implemented during in-line manufacturing to maintain quality at each stage of operations. In this study, a mid-infrared (MIR) quantum cascade laser (QCL) spectroscopy-based protocol was performed to quantify ibuprofen in formulations of powder blends and tablets. Fourteen blends were prepared with varying concentrations from 0.0% to 21.0% (w/w) API. MIR laser spectra were collected in the spectral range of 990 to 1600 cm−1. Partial least squares (PLS) models were developed to correlate the intensities of vibrational signals with API concentrations in powder blends and tablets. PLS models were evaluated based on the following figures of merit: correlation coefficient (R2), root mean square error of calibration, root mean square error of prediction, root mean square error of cross-validation, and relative standard error of prediction. QCL assisted by multivariate analysis was demonstrated to be accurate and robust for analysis of the content and blend uniformity of pharmaceutical compounds.
Highlights
The RMSECV and RMSEP values obtained for the quantum cascade laser (QCL)–Partial least squares (PLS) tablet and powder models using D3 are lower than D1 and D2. These results show that D3 contains a broader spectral region than the other two diodes, corresponding to more molecular information in the active pharmaceutical ingredients (APIs)’s vibrational signals
Sudden changes in the process will be detectable with this system, considering that the system requires only 1.5 s to acquire a spectrum
The MIR region provides a unique absorption spectrum for different components; it enables the detection of polymorphic transformation
Summary
The development of analytical methods requiring minimal, or no sample preparation, a short analysis time, and high sensitivity is fundamental to minimizing specification products. The traditional analytical methods for quantifying active pharmaceutical ingredients (API) include chromatographic [1,2,3,4] and optical techniques (UV–Vis) [5,6,7]. These methods have high reproducibility and low detection limits, they involve destroying the samples or transporting them to the laboratory for further analysis.
Sign-in/Register to view highlights & summary Sign-in/Register to access full text options 
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
