Multivariate Chemometric Approach to Thermal Solid-State FT-IR Monitoring of Pharmaceutical Drug Compound

Tan, Wei Chit; Widjaja, Effendi

doi:10.1002/jps.21275

“…Hot stage Hot-stage Raman and NIR spectroscopy TPS, NIR and Raman spectroscopy Lisinopril [136] Dehydrate formation of lisinopril dihydrate Hot stage…”

Section: Raman Spectroscopymentioning

confidence: 99%

“…A different multivariate method -self-modelling curve resolution -was used to quantify multiple forms of lisinopril during its dehydration. [136] Another recent study using variable-temperature TPS investigated differences in the terahertz spectra of anhydrous and hydrated APIs, including lactose, piroxicam, carbamazepine and theophylline, and also analysed the dehydration of theophylline monohydrate in situ between 293 and 437 K. [81] The anhydrous and hydrated forms of the different APIs could be easily distinguished using TPS. The dehydration experiment on theophylline monohydrate revealed that in-situ TPS is a valuable technique for studying dehydration and water evaporation processes and mechanisms in pharmaceutical materials.…”

Section: Raman Spectroscopymentioning

confidence: 99%

“…In-situ NIR and Raman spectroscopy Erythromycin A [132][133][134] [82,135] Dehydrate formation of piroxicam monohydrate Hot stage Hot-stage Raman and NIR spectroscopy TPS, NIR and Raman spectroscopy Lisinopril [136] Dehydrate formation of lisinopril dihydrate Hot stage In-situ IR spectroscopy Lactose, piroxicam, carbamazepine, theophylline [81] Dehydrate formation of lactose a-monohydrate piroxicam monohydrate, carbamazepine dihydrate and theophylline dihydrate Hot stage In-situ TPS Ampicillin, nitrofurantoin, besylate salt of compound A [137] Hydrate formation Storage IR spectroscopy Niclosamide [138] Hydrate and dehydrate formation Humidity cell Raman spectroscopy API, active pharmaceutical ingredient; IR, infrared; NIR, near infrared; TPS, terahertz pulsed spectroscopy.…”

Section: Fluid-bed Drying and Experiments On A Hot Stagementioning

confidence: 99%

See 1 more Smart Citation

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Heinz

¹

,

Strachan

²

,

Gordon

³

et al. 2009

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Objectives Solid-state transformations may occur during any stage of pharmaceutical processing and upon storage of a solid dosage form. Early detection and quantification of these transformations during the manufacture of solid dosage forms is important since the physical form of an active pharmaceutical ingredient can significantly influence its processing behaviour, including powder flow and compressibility, and biopharmaceutical properties such as solubility, dissolution rate and bioavailability. Key findings Vibrational spectroscopic techniques such as infrared, near-infrared, Raman and, most recently, terahertz pulsed spectroscopy have become popular for solidstate analysis since they are fast and non-destructive and allow solid-state changes to be probed at the molecular level. In particular, Raman and near-infrared spectroscopy, which require no sample preparation, are now commonly used coupled to fibreoptic probes and are able to characterise solid-state conversions in-line. Traditionally, uni-or bivariate approaches have been used to analyse spectroscopic data sets; however, recently the simultaneous detection of several solid-state forms has been increasingly performed using multivariate approaches where even overlapping spectral bands can be analysed. Summary This review discusses the applications of different vibrational spectroscopic techniques to detect and monitor solid-state transformations possible for crystalline polymorphs, hydrates and amorphous forms of pharmaceutical compounds. In this context, the theoretical basis of solid-state transformations and vibrational spectroscopy and common experimental approaches are described, including recent methods of data analysis.

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“…Mid‐IR spectroscopy, which is sensitive to both solid‐state form and the presence of water, was used to analyse drug dehydration on a hot stage using a microscope setup in transmission mode. A different multivariate method – self‐modelling curve resolution – was used to quantify multiple forms of lisinopril during its dehydration 136 . Another recent study using variable‐temperature TPS investigated differences in the terahertz spectra of anhydrous and hydrated APIs, including lactose, piroxicam, carbamazepine and theophylline, and also analysed the dehydration of theophylline monohydrate in situ between 293 and 437 K 81 .…”

Section: Introductionmentioning

confidence: 99%

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Heinz

¹

,

Strachan

²

,

Gordon

³

et al. 2009

Journal of Pharmacy and Pharmacology

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Objectives Solid-state transformations may occur during any stage of pharmaceutical processing and upon storage of a solid dosage form. Early detection and quantification of these transformations during the manufacture of solid dosage forms is important since the physical form of an active pharmaceutical ingredient can significantly influence its processing behaviour, including powder flow and compressibility, and biopharmaceutical properties such as solubility, dissolution rate and bioavailability. Key findings Vibrational spectroscopic techniques such as infrared, near-infrared, Raman and, most recently, terahertz pulsed spectroscopy have become popular for solidstate analysis since they are fast and non-destructive and allow solid-state changes to be probed at the molecular level. In particular, Raman and near-infrared spectroscopy, which require no sample preparation, are now commonly used coupled to fibreoptic probes and are able to characterise solid-state conversions in-line. Traditionally, uni-or bivariate approaches have been used to analyse spectroscopic data sets; however, recently the simultaneous detection of several solid-state forms has been increasingly performed using multivariate approaches where even overlapping spectral bands can be analysed. Summary This review discusses the applications of different vibrational spectroscopic techniques to detect and monitor solid-state transformations possible for crystalline polymorphs, hydrates and amorphous forms of pharmaceutical compounds. In this context, the theoretical basis of solid-state transformations and vibrational spectroscopy and common experimental approaches are described, including recent methods of data analysis.

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“…In addition, the "accelerated shelf-life estimation" for various pharmaceuticals has also been explored, in both solution, e.g., [13,14], and solid, e.g., [15][16][17], phases. However, the studies we report herein are unique in both the range of experimental conditions that are explored and the types of kinetics that are observed/modeled/interpreted, under these conditions.…”

Section: Introductionmentioning

confidence: 99%

Use of real‐time FT‐IR monitoring of a pharmaceutical compound under stress atmospheric conditions to characterize its solid‐state degradation kinetics

Skrdla

¹

,

Harrington

²

,

Lin

³

2009

Int J of Chemical Kinetics

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The use of online FT-IR is described for investigating the degradation kinetics of the solid amorphous pharmaceutical compound, fosaprepitant dimeglumine (FD), under stress storage conditions (i.e., high temperature, T, and humidity, % RH). It is found that under conditions of elevated T and % RH, the kinetics are denucleation rate limited for the deliquescence of the amorphous FD solid, based on the high quality fits obtained to the authors' dispersive kinetic model for that mechanism. At elevated T and low % RH, it is found that a classical, first-order hydrolysis mechanism for the degradation of FD (which forms crystalline aprepitant, AP) significantly contributes to the overall conversion rate. That mechanism is similar to the one observed previously for the solution-phase hydrolysis of FD. Appropriate kinetic models are proposed for the FD-to-AP conversion under all of the experimental conditions investigated in this work. C 2009 Wiley Periodicals, Inc. Int J Chem Kinet 42: 25

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Multivariate Chemometric Approach to Thermal Solid-State FT-IR Monitoring of Pharmaceutical Drug Compound

Cited by 11 publications

References 19 publications

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Analysis of solid-state transformations of pharmaceutical compounds using vibrational spectroscopy

Use of real‐time FT‐IR monitoring of a pharmaceutical compound under stress atmospheric conditions to characterize its solid‐state degradation kinetics

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