Feasibility of near Infrared Chemical Imaging for Pharmaceutical Cleaning Verification

Abstract

In conformity with the 2011 Food and Drug Administration guidance for industry, Process Validation: General Principles and Practices, there is a requirement for new methodologies that support continued cleaning verification of manufacturing equipment. Near infrared chemical imaging (NIR-CI) represents an attractive alternative to the current methodologies for cleaning verification since it represents a direct, rapid and sensitive technology. The aim of this study was to test the feasibility of NIR-CI for cleaning verification. Stainless steel, glass and Perspex surfaces were soiled with selected active pharmaceutical ingredients (APIs) with the resulting hyperspectral data employed to identify and quantify the dried residues. Correlations to high-performance liquid chromatography (HPLC) swab analysis were also made. Linear models were obtained for the number of API classified pixels and applied soil concentration with R 2 values of 0.90 and 0.98 for caffeine and sulfathiazole sodium salt, respectively, on stainless steel coupons. In the case of caffeine soils on borosilicate glass and Perspex coupons, the obtained R 2 values were 0.95 and 0.96, respectively. These R 2 values suggest a linear relationship between the number of API classified pixels and applied soil concentration. The calculated detection limits for caffeine and sulfathiazole sodium salt soils on stainless steel coupons were 48 µg and 18 µg 50 mm −2 , respectively. For caffeine soils on borosilicate glass and Perspex coupons the calculated detection limits were 33 µg and 27 µg 50 mm −2 , respectively. However, visual inspection of the NIR-CI following the classification function point to limits of detection closer to 1 µg 50 mm −2 or lower. High correlations (R 2 of 0.91 and 0.93 for caffeine and sulfathiazole sodium salt, respectively) were also obtained between NIR-CI API soil quantification and swabbing/ HPLC analysis. This research points to possible future use of portable CI systems for continued cleaning verification of pharmaceutical residues.

Recent Progress of Near-Infrared (NIR) Imaging —Development of Novel Instruments and Their Applicability for Practical Situations—

“…4,9,[25][26][27][28][29][30] In polymer science and technology it has been used to investigate the phase separation, miscibility, and morphology of polymer blends. [31][32][33] With this technique, researchers can easily obtain information about the distribution of different components or the different polymer morphologies in blends.…”

Quality Assurance of Torrefied Biomass Using RGB, Visual and near Infrared (Hyper) Spectral Image Data

“…The reorganization results in a data structure where the pixels become observations, and the wavelengths become variables. Several papers, where hyperspectral imaging has been combined with chemometrics , have been published within the fields of food, 23-27 pharmaceutical [28][29][30][31][32][33] and polymer research. 34,35 Biomass applications of hyperspectral imaging in the laboratory have been published.…”

Novel Cleaning-in-Place Strategies for Pharmaceutical Hot Melt Extrusion

“…Several analytical techniques have been reported in the literature, including total organic carbon (TOC) [10], ion mobility spectroscopy [11][12][13][14], mass spectrometry [15,16] and more recently a light induced fluorescence sensor for at-line CV [17]. Furthermore, near infrared (NIR) chemical imaging was shown to be suitable for CV of various surface materials [18]. These methods have advantages over the classical rinse and swab/HPLC approach, since they require considerably less time and/or can potentially eliminate the prerequisite of swabbing/rinsing.…”