The use of near-infrared spectroscopy in the efficient prediction of a specification for the residual moisture content of a freeze-dried product

Derksen, Marco W.J.; Oetelaar, Piet J.M. van de; Maris, F.A.

doi:10.1016/s0731-7085(97)00216-1

Cited by 56 publications

(28 citation statements)

References 5 publications

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“…In solid-state analysis, NIR spectroscopy has been applied for identification and quantification of polymorphs and amorphous forms in powder mixtures and solid dosage forms such as tablets. [44][45][46][47][48][49][50][51] It has been also used for several process analytical applications, such as moisture detection during wet granulation, [52][53][54] in freezedried solids, [55] and to describe crystallisation processes. [56] NIR spectroscopy has also become important in the study of solid-state transformations (described below).…”

Section: Near-infrared Spectroscopymentioning

confidence: 99%

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

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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Section: Near-infrared Spectroscopymentioning

confidence: 99%

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

et al. 2009

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“…These characteristics ensure that an entire batch can be thoroughly examined without modifying the content of vials. Over the last twenty years, several reports have been published concerning the determination of moisture content of lyophilized products by scanning through the bottom of vials (Kamat et al, 1989;Zheng et al, 2008;Derksen et al, 1998;Stokvold et al, 2002). Nonetheless, these studies have focused on development of models for accurate and precise at-line determinations by means of conventional spectrometers.…”

Section: Introductionmentioning

confidence: 99%

Determination of moisture content in lyophilized mannitol through intact glass vials using NIR micro-spectrometers

Muzzio

Dini²,

Simionato

2011

Braz. J. Pharm. Sci.

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Determination of moisture content in lyophilized solids is fundamental to predict quality and stability of freeze-dried products, but conventional methods are time-consuming, invasive and destructive. The aim of this study was to develop and optimize a fast, inexpensive, noninvasive and nondestructive method for determination of moisture content in lyophilized mannitol, based on an NIR micro-spectrometer instead of a conventional NIR spectrometer. Measurements of lyophilized mannitol were performed through the bottom of rotating glass vials by means of a reflectance probe. The root mean standard error of prediction (RMSEP) and the correlation coefficient (R 2 pred ), yielded by the pre-treatments and calibration method proposed, was 0.233% (w/w) and 0.994, respectively.Uniterms: Near-infrared spectroscopy. Lyophilization. Multivariate analysis. Moisture content. Mannitol. Micro-spectrometer.A determinação do conteúdo de umidade em sólidos liofilizados é fundamental para se prever a qualidade e a estabilidade de produtos liofilizados, mas os métodos convencionais consomem muito tempo, são invasivos e destrutivos. O objetivo desse estudo foi desenvolver e otimizar um método rápido, econômico, não invasivo e não destrutivo para a determinação do conteúdo de umidade em manitol liofilizado, com base em microespectrômetro de infravermelho próximo ao invés de um espectrômetro de infravermelho próximo convencional. As medidas de manitol liofilizado foram realizadas através do fundo de recipiente de vidro em rotação por meio de sonda de reflectância. A raíz do erro médio padrão de predição (RMSEP) e o coeficiente de correlação (R 2 pred ) obtidos pelo prétratamento e pelo método de calibração proposto foram, respectivamente, 0,233% (p/p) e 0,994. Uniterms: Espectroscopia de infravermelho próximo. Liofilização. Análise multivariada. Análise de unidade. Manitol. Microespectrômetro.

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“…In early publications Derksen [5] and Kamat [6] found a good correlation between the amount of water analysed with NIR and Karl-Fischer titration using large ranges of the NIR spectrum. Recently, narrower ranges of the spectra have been used to describe the state of water.…”

Section: Introductionmentioning

confidence: 99%

Classification of lyophilised mixtures using multivariate analysis of NIR spectra

Grohganz

Fonteyne

Skibsted

et al. 2010

European Journal of Pharmaceutics and Biopharmaceutics

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Excipient selection is critically affecting the processing and the stability of a lyophilised product. Near infra-red (NIR) spectroscopy was applied to investigate freeze-dried samples containing varying ratios of the commonly used excipients mannitol and sucrose.Further variation in the formulation was achieved by adding NaCl, CaCl 2 and histidine and by exposing the samples to different conditions. Untreated NIR spectra are strongly affected by the physical nature of samples and can thus be useful for detecting production outliers. Applying standard normal variate (SNV) transformation highlights chemical information. The obtained NIR spectra of the freeze-dried samples were clustered by principal component analysis (PCA) after applying SNV correction in the range 4200 to 7400 cm -1 (1350 2380 nm). Relative humidity under storage and the mannitol-sucrose ratio were clearly represented in the first two principal components, while influence of other excipients was observed in the 3 rd and 4 th principal component. It was investigated whether this could be due to an influence of the excipients on the mannitol crystallisation behaviour. Performing PCA with 2 principal components of SNV-corrected spectra in the range 4200 4500 cm -1 (2220 1380 nm) led to the following observation: While the 1 st principal component closely resembled the spectra of b-mannitol, the 2 nd principal component contained additional features that were not attributable to b-mannitol but correlated well to the main absorbance band of d-mannitol and mannitol hemihydrate.Therefore, it seems feasible that NIR can analyse versatile freeze-dried samples and classify these according to composition, water content and solid-state properties.

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The use of near-infrared spectroscopy in the efficient prediction of a specification for the residual moisture content of a freeze-dried product

Cited by 56 publications

References 5 publications

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

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

Determination of moisture content in lyophilized mannitol through intact glass vials using NIR micro-spectrometers

Classification of lyophilised mixtures using multivariate analysis of NIR spectra

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