Application of Diffuse Reflectance Near‐Infrared Spectroscopy for Determination of Crystallinity

Seyer, Jeffery J.; Luner, Paul E.; Kemper, Mark S.

doi:10.1002/1520-6017(200010)89:10<1305::aid-jps8>3.0.co;2-q

Cited by 56 publications

(16 citation statements)

References 35 publications

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“…In addition, further quantitative information can be extracted from the data using chemoinfometrics, where the collected data is processed by means of statistical and applied mathematical techniques. Quantification of crystallinity is usually performed using the first (140) or second derivate spectra (95,141,142). Physical and chemical information such as polymorphism (143) and mutarotation (144) may be obtained.…”

Section: Near Infrared Spectroscopymentioning

confidence: 87%

Methods of amorphization and investigation of the amorphous state

Einfalt¹,

Planinšek²,

Hrovat³

2013

Acta Pharmaceutica

117

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.g., polymorphs) provides pharmaceutical scientists with an opportunity to select the preferred form of the material to be used in a formulation. This is very useful since critical properties, such as particle morphology and dissolution properties, are frequently different in the different physical forms of a material. The amorphous form of pharmacologically active materials has received considerable attention because, in theory, it represents the most energetic solid state of a material, and should thus provide the biggest advantages in terms of dissolution rate and bioavailability (1). However, the amorphous form also shows various disadvantages, such as lower physical stability compared to crystals.The structure of an amorphous solid is usually described as possessing a crystal--like short-range molecular arrangement, but lacking a long-range order. As illustrated by Fig. 1, the immediate environment of a molecule (m) in an amorphous solid may not differ significantly from that in a crystal (e.g., similar number of and distance to nearest neighbors), but an amorphous solid lacks any long-range transational-orientational symmetry that characterizes a crystal (1). However, this is only true when we are dealing The amorphous form of pharmaceutical materials represents the most energetic solid state of a material. It provides advantages in terms of dissolution rate and bioavailability. This review presents the methods of solid--state amorphization described in literature (supercooling of liquids, milling, lyophilization, spray drying, dehydration of crystalline hydrates), with the emphasis on milling. Furthermore, we describe how amorphous state of pharmaceuticals differ depending on the method of preparation and how these differences can be screened by a variety of spectroscopic (X-ray powder diffraction, solid state nuclear magnetic resonance, atomic pairwise distribution, infrared spectroscopy, terahertz spectroscopy) and calorimetry methods.

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Section: Near Infrared Spectroscopymentioning

confidence: 87%

Methods of amorphization and investigation of the amorphous state

Einfalt¹,

Planinšek²,

Hrovat³

2013

Acta Pharmaceutica

117

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“…MLR predicted a crystallinity   of 0.99 for the mixtures of crystalline and amorphous lactose, which indicated that NIR can determine the crystallinity of materials during pharmaceutical manufacturing. Seyer et al (2000) conducted a study on the identification of the degree of crystallinity in powder mixtures of sucrose and indomethacin using diffuse reflectance NIR spectroscopy (1100-2500 nm). This study also used XRD and DSC methods for parallel studies of the mixtures.…”

Section: Polymorphismmentioning

confidence: 99%

Spectroscopic Techniques for Nondestructive Quality Inspection of Pharmaceutical Products: A Review

Kandpal

Park

Tewari

et al. 2015

Journal of Biosystems Engineering

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Spectroscopy is an emerging technology for the quality assessment of pharmaceutical samples, from tablet manufacturing to final quality assurance. The traditional methods for the quality management of pharmaceutical tablets are time consuming and destructive, while spectroscopic techniques allow rapid analysis in a non-destructive manner. The advantage of spectroscopy is that it collects both spatial and spectral information (called hyperspectral imaging), which is useful for the chemical imaging of pharmaceutical samples. These chemical images provide both qualitative and quantitative information on tablet samples. In the pharmaceutics, spectroscopic techniques are used for a variety of applications, such as analysis of the homogeneity of powder samples as well as determination of particle size, product composition, and the concentration, uniformity, and distribution of the active pharmaceutical ingredient in solid tablets. This review paper presents an introduction to the applications of various spectroscopic techniques such as hyperspectroscopy and vibrational spectroscopies (Raman spectroscopy, FT-NIR, and IR spectroscopy) for the quality and safety assessment of pharmaceutical solid dosage forms. In addition, various chemometric techniques that are highly essential for analyzing the spectroscopic data of pharmaceutical samples are also reviewed.

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“…Finally, a new model was generated from a combination of the original and restricted calibrations, leading to: R-SEC = 0.117% (w/w); calibration slope = 0.992; calibration intercept = 0.0174; R 2 Cal = 0.996; RMSEP = 0.233% (w/w); RSEP = 8.21% (w/w); prediction slope = 0.944; prediction intercept = 0.0147; R 2 Pred = 0.994. The limit of detection (LOD) and LOQ were estimated by calculating the standard deviation (SD) of samples from the calibration and validation sets with moisture content close to the LOD and LOQ (range was selected iteratively) and multiplying each SD by 3 and 10, respectively (Patel et al, 2001;Seyer et al, 2000). This estimation provides an approximate LOD value of 0.22% (w/w) and LOQ value of 0.73% (w/w).…”

Section: Model Assessmentmentioning

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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Application of Diffuse Reflectance Near‐Infrared Spectroscopy for Determination of Crystallinity

Cited by 56 publications

References 35 publications

Methods of amorphization and investigation of the amorphous state

Methods of amorphization and investigation of the amorphous state

Spectroscopic Techniques for Nondestructive Quality Inspection of Pharmaceutical Products: A Review

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

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