Figures of Merit Comparison of Reflectance and Transmittance Near-Infrared Methods for the Prediction of Constituent Concentrations in Pharmaceutical Compacts

Abstract

The purpose of this work was to demonstrate how multivariate figures of merit, in conjunction with accuracy and precision statistics, can be used to evaluate the performance of near-infrared reflectance and transmittance spectroscopy for the nondestructive chemical quantification of intact pharmaceutical compacts. A total of 174 four-component compacts were produced at five compaction pressures following a fully balanced quaternary design. Near-infrared spectra were measured in both reflectance and transmittance modes. Partial least-squares regression was used to model spectroscopic response, and net analyte signal theory was used to generate the figures of merit. It was discovered that sample positioning variation more negatively impacted the performance (analytical sensitivity, S/N ratio, limit of detection) of the transmittance method. Process analytical technology implementation teams should consider these aspects during technology selection, method development, and validation.

A Near-Infrared Spectroscopic Investigation of Relative Density and Crushing Strength in Four-Component Compacts

“…When concentration is held constant, both relative density and crushing strength are modeled well by the standard deviation of the log(1/ R ) spectra. The authors suggest that the thickness of the compacts (mean = 4.387 mm, median = 4.307 mm, standard deviation = 0.237 mm, n = 174) in conjunction with tablet positioning error32 may have compromised the integrity of the transmittance results due to nonlinearity.…”

Effects and Detection of Raw Material Variability on the Performance of Near-Infrared Calibration Models for Pharmaceutical Products

“…The materials were mixed in 25 mL glass scintillation vials for 10 min by placing them on the rotating drive assembly of a Jar Mill (US Stoneware, East Palestine, Ohio). The blending time was chosen in accordance with a previous study that used a NIR‐based prediction approach to estimate the homogeneity of similar blends . The mixtures from each design point were then subdivided and compacted at two of five pressures (67.0, 117.3, 167.6, 217.8, and 268.1 MPa), randomly selected, on a Carver Automatic Tablet Press (Model 3887.1SD0A00; Wabash, Indiana) using a 13‐mm die and flat‐faced punches.…”

Feasibility Study of Diffuse Reflectance and Transmittance near Infrared Spectroscopy for Rapid Analysis of Ascorbic Acid Concentration in Bilayer Tablets Using a High-Speed Polychromator-Type Spectrometer

“…Similar results have been reported in other studies where the FT-type and monochromator-type spectrometers and longer spectral-scanning times have been adopted. 14,18,19,24,27 Figure 5 shows the second-derivative DR-NIR spectra of the bilayer tablet and their expansion in the 1440-1480 nm region. The second-derivative spectra are spiky because of the high Table 1.…”

“…[11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26][27][28] The advantages of diffuse reflectance (DR) and transmittance (Tr) spectral-acquisition methods have been reported. [18][19][20][21][22][23][24][25] The advantages and disadvantages of both methods can be summarised as follows: the DR-NIR method is robust against sample positioning errors, which is advantageous for online NIR measurements. For the analysis of tablets, the DR-NIR spectra allows the utilisation of a wide region of wavelength, while a spectral range with wavelengths greater than 1400 nm is unavailable in the Tr-NIR spectra.…”

“…As mentioned above, the analysis of tablets by NIR spectroscopy has been extensively researched. Most of the research was performed for laboratory use with the help of Fourier-transform and monochromator-type spectrometers; [12][13][14][15][16][18][19][20][21][23][24][25][26][27][28] in some cases, portable NIR spectrometers were used. 17,22 Generally, the spectra obtained from laboratory-use spectrometers have high signal-to-noise ratios (SNR).…”