Raman spectroscopy for the qualitative and quantitative analysis of solid dosage forms of Sitagliptin

Bakkar, Muhammad Abu; Nawaz, Haq; Majeed, Muhammad Irfan; Naseem, Ammara; Ditta, Allah; Rashid, Nosheen; Ali, Saqib; Bajwa, Jawad; Bashir, Saba; Ahmad, Shamsheer; Hyat, Hamza; Bukhari, Kareem Shah; Bonnier, Franck

doi:10.1016/j.saa.2020.118900

Cited by 44 publications

(30 citation statements)

References 25 publications

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“…Figure a shows the Raman spectra of SIT powder and SIT solution, labeled with vertical lines and the corresponding peak assignments. The spectral features of SIT were previously reported . The Raman peaks observed at 726, 748, 759, and 881 cm –1 correspond to C–F symmetric stretching vibrations, with C–C alkyl chain stretching at 1077 cm –1 , C–H 2 wagging at 1340 cm –1 , aromatic ring CC stretching at 1520 cm –1 , and a CO stretching vibration 1634 cm –1 .…”

Section: Resultssupporting

confidence: 57%

Understanding the Adsorption and Desorption of Sitagliptin Phosphate Monohydrate on SS2343, Glass, and PTFE Using QCM-D and Raman Spectroscopy

et al. 2022

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Cross-contamination during pharmaceutical drug manufacturing can result in expensive recalls. To counter that, companies spend significant time and resources to ensure equipment cleanliness, often relying on the compound solubility data in various solvents as the main indicator of cleaning success. The aim of this work is to provide an alternative way to analyze the fouling and cleaning of surfaces in pharmaceutical manufacturing processes by using the quartz crystal microbalance with dissipation (QCM-D) and Raman spectroscopy. In this study, we chose an active pharmaceutical ingredient (API), sitagliptin phosphate monohydrate (SIT), as the model drug compound and observed its adsorption and desorption on stainless steel (SS2343), borosilicate glass (glass), and polytetrafluoroethylene (PTFE) surfaces. SIT was selected as the model API since it is a product manufactured on a large scale and is part of the widely used dipeptidyl peptidase-IV inhibitor class of oral hypoglycemics used to treat type 2 diabetes mellitus, while the chosen surfaces mimic the wall materials of manufacturing equipment and components such as reactors, transfer lines, and valves. Both the QCM-D and Raman spectroscopy results show the highest physisorption on PTFE, followed by SS2343 and glass. Additionally, QCM-D revealed a harder removal of SIT from SS2343 compared to glass and PTFE. Raman analysis of the chemical interactions disclosed C−F and C�O bond interactions between SIT and the surfaces, and the lack of a peak shift suggested dipole−dipole interactions. Furthermore, contact angle measurements indicate that hydrophobic attraction contributed to SIT adhesion to the PTFE surface. Subsequently, SIT coverage upon deposition on a PTFE surface has a significantly smaller surface area than on SS2343 and glass due to surface hydrophobicity, hence resulting in a longer removal time. These results provide a practical use of QCM-D and Raman spectroscopy to enhance the understanding of fouling and improve the cleaning of complex small molecules on relevant surfaces during the pharmaceutical manufacturing process.

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Section: Resultssupporting

confidence: 57%

Understanding the Adsorption and Desorption of Sitagliptin Phosphate Monohydrate on SS2343, Glass, and PTFE Using QCM-D and Raman Spectroscopy

et al. 2022

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“…More recently, a study using Raman cartography highlighted that hydrophobic compounds from Punica granatum seed oil hydroxyphenethyl esters (PHE) stabilised in a poloxamer-based nanosystem showed very homogeneous distribution in hydrophilic PVA films compared to the free form introduced as an ethanol solution [14]. While quantitative analysis of AI concentrations in cosmetic and pharmaceutical products using Raman spectroscopy is increasingly documented for solutions and semi-solids forms (gels, cream) [29][30][31], application of the technique to solid complex mixtures remains largely limited to semi-quantitative analysis [32][33][34].…”

Section: Introductionmentioning

confidence: 99%

Confocal Raman Spectroscopic Imaging for Evaluation of Distribution of Nano-Formulated Hydrophobic Active Cosmetic Ingredients in Hydrophilic Films

et al. 2021

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Film-forming systems are highly relevant to the topical administration of active ingredients (AI) to the body. Enhanced contact with the skin can increase the efficacy of delivery and penetration during prolonged exposure. However, after the evaporation of volatile solvents to form a thin film, the distribution of the ingredient should remain homogenous in order to ensure the effectiveness of the formula. This is especially critical for the use of hydrophobic molecules that have poor solubility in hydrophilic films. In order to address this concern, hydroxyphenethyl esters (PHE) of Punica granatum seed oil were prepared as a nanosuspension stabilised by poloxamers (NanoPHE). NanoPHE was then added to a formulation containing polyvinyl alcohol (PVA) as a film forming agent, Glycerol as a plasticiser and an antimicrobial agent, SepicideTM HB. Despite their reliability, reference methods such as high-performance liquid chromatography are increasingly challenged due to the need for consumables and solvents, which is contrary to current concerns about green industry in the cosmetics field. Moreover, such methods fail to provide spatially resolved chemical information. In order to investigate the distribution of ingredients in the dried film, Confocal Raman imaging (CRI) coupled to Non-negatively Constrained Least Squares (NCLS) analysis was used. The reconstructed heat maps from a range of films containing systematically varying PHE concentrations highlighted the changes in spectral contribution from each of the ingredients. First, using NCLS scores it was demonstrated that the distributions of PVA, Glycerol, SepicideTM HB and PHE were homogenous, with respective relative standard deviations (RSD) of 3.33%, 2.48%, 2.72% and 6.27%. Second, the respective relationships between ingredient concentrations in the films and their Raman responses, and the spectral abundance were established. Finally, a model for absolute quantification for PHE was be constructed using the percentage of spectral abundance. The prepared %w/w concentrations regressed against predicted %w/w concentrations, displaying high correlation (R2 = 0.995), while the Root Mean Squared Error (0.0869% w/w PHE) confirmed the precision of the analysis. The mean percent relative error of 3.75% indicates the accuracy to which the concentration in dried films could be determined, further supporting the suitability of CRI for analysis of composite solid film matrix. Ultimately, it was demonstrated that nanoformulation of hydrophobic PHE provides homogenous distribution in PVA based film-forming systems independent of the concentration of NanoPHE used in the formula.

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“…In various scientific fields of research, it is necessary to analyze materials’ structural and electronic properties. Scientists have developed various qualitative and quantitative analytic methods, including Raman and photoluminescence (PL) spectroscopies [ 1 , 2 , 3 ]. The Raman effect is an inelastic photon scattering process in which a transfer of energy between the light and the system corresponds to the energy of a particular vibrational state of the material.…”

Section: Introductionmentioning

confidence: 99%

Raman and Photoluminescence Spectroscopy with a Variable Spectral Resolution

Pavić

Šoda

Gašparić

et al. 2021

Sensors

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Raman and photoluminescence (PL) spectroscopy are important analytic tools in materials science that yield information on molecules’ and crystals’ vibrational and electronic properties. Here, we show results of a novel approach for Raman and PL spectroscopy to exploit variable spectral resolution by using zoom optics in a monochromator in the front of the detector. Our results show that the spectral intervals of interest can be recorded with different zoom factors, significantly reducing the acquisition time and changing the spectral resolution for different zoom factors. The smallest spectral intervals recorded at the maximum zoom factor yield higher spectral resolution suitable for Raman spectra. In contrast, larger spectral intervals recorded at the minimum zoom factor yield the lowest spectral resolution suitable for luminescence spectra. We have demonstrated the change in spectral resolution by zoom objective with a zoom factor of 6, but the perspective of such an approach is up to a zoom factor of 20. We have compared such an approach on the prototype Raman spectrometer with the high quality commercial one. The comparison was made on ZrO2 and TiO2 nanocrystals for Raman scattering and Al2O3 for PL emission recording. Beside demonstrating that Raman spectrometer can be used for PL and Raman spectroscopy without changing of grating, our results show that such a spectrometer could be an efficient and fast tool in searching for Raman and PL bands of unknown materials and, thereafter, spectral recording of the spectral interval of interest at an appropriate spectral resolution.

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Raman spectroscopy for the qualitative and quantitative analysis of solid dosage forms of Sitagliptin

Cited by 44 publications

References 25 publications

Understanding the Adsorption and Desorption of Sitagliptin Phosphate Monohydrate on SS2343, Glass, and PTFE Using QCM-D and Raman Spectroscopy

Understanding the Adsorption and Desorption of Sitagliptin Phosphate Monohydrate on SS2343, Glass, and PTFE Using QCM-D and Raman Spectroscopy

Confocal Raman Spectroscopic Imaging for Evaluation of Distribution of Nano-Formulated Hydrophobic Active Cosmetic Ingredients in Hydrophilic Films

Raman and Photoluminescence Spectroscopy with a Variable Spectral Resolution

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