Development of an analytical method for crystalline content determination in amorphous solid dispersions produced by hot-melt extrusion using transmission Raman spectroscopy: A feasibility study

Netchacovitch, Lauranne; Dumont, Elodie; Cailletaud, Johan; Thiry, Justine; Bleye, Charlotte De; Sacré, Pierre-Yves; Boiret, Mathieu; Évrard, Brigitte; Hubert, Ph.; Ziemons, Eric

doi:10.1016/j.ijpharm.2017.07.052

Cited by 28 publications

(15 citation statements)

References 32 publications

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“…Solvation states and polymorphic forms have been extensively studied using Raman based technologies [15,16]. There are a few notable examples that utilise TRS; initial work showed the expected benefit of superior quantification compared to backscatter geometries [17,18]. Further work compared TRS to NIR, with TRS achieving marginally better quantitative model performance statistics [19].…”

Section: Transmission Raman Spectroscopymentioning

confidence: 99%

Quantifying low levels (<0.5% w/w) of warfarin sodium salts in oral solid dose forms using Transmission Raman spectroscopy

Griffen

Owen

Matousek

2018

Journal of Pharmaceutical and Biomedical Analysis

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In this feasibility study Transmission Raman spectroscopy (TRS) has been used to build quantitative models for warfarin sodium and warfarin sodium clathrate. The type of warfarin present in manufactured tablets may affect product quality. Models were used to predict warfarin sodium in commercially available tablets at extremely low dosage levels (0.5% w/w). The laboratory made calibration samples used in the modelling varied in amorphous sodium, crystalline clathrate warfarin forms, excipients and dye. This application was highly challenging due to the low level of API and high level of a Raman-active colourant which varied significantly between production batches. A photon recycling optic, known as a Beam Enhancer, was utilised to improve the signal to noise of the Raman spectra to attain a low limit of quantification of 0.19% w/w.

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Section: Transmission Raman Spectroscopymentioning

confidence: 99%

Quantifying low levels (<0.5% w/w) of warfarin sodium salts in oral solid dose forms using Transmission Raman spectroscopy

Griffen

Owen

Matousek

2018

Journal of Pharmaceutical and Biomedical Analysis

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“…Netchacovitch et al used Raman spectroscopy to determine crystalline itraconazole in amorphous solid dispersions prepared by hotmelt extrusion. Calibration set included three levels of concentration and was built by using crystalline API powder, six batches of grinded extrudates with amorphous API, and placebogrinded extrudate [25].…”

Section: Different Levels Of the Investigated Propertymentioning

confidence: 99%

“…It was demonstrated that the prediction accuracy was influenced only by relative humidity, generating a positive bias in samples stored at 50%RH. Therefore, the entire calibration and validation was reconsidered by pre-conditioning the samples at 25 C and 50%RH for 20 h, prior to recording the spectra and building the model. This way, the robustness of the method was increased to future expected variations in environmental conditions [21].…”

Section: Different Levels Of the Investigated Propertymentioning

confidence: 99%

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Multivariate Calibration for the Development of Vibrational Spectroscopic Methods

Tomuță¹,

Porfire²,

Casian³

et al. 2018

Calibration and Validation of Analytical Methods - A Sampling of Current Approaches

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Vibrational spectroscopy, namely near infrared (NIR) and Raman spectroscopy, is based on the interaction between the electromagnetic radiation and matter. The technique is sensitive to chemical and physical properties and delivers a wide range of information about the analyzed sample, but in order to extract the information, multivariate calibration of the spectral data is required. The main goal of this work will be to present in detail the available multivariate calibration strategy for development of NIR and Raman spectroscopic methods, which was successfully applied in pharmaceutics.

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“…Twin-screw hot melt extrusion (HME) is a continuous process that has been widely used to enhance the solubility of active pharmaceutical ingredients (APIs) [1,2]. This process applies heat and shear energy to produce an amorphous solid dispersion (ASD) of an API into a polymer carrier [3,4]. As a continuous process, HME has the potential to be used in combination with in-line analytical techniques to enable real time monitoring of product quality.…”

Section: Introductionmentioning

confidence: 99%

Development and Validation of an in-line API Quantification Method Using AQbD Principles Based on UV-Vis Spectroscopy to Monitor and Optimise Continuous Hot Melt Extrusion Process

et al. 2020

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A key principle of developing a new medicine is that quality should be built in, with a thorough understanding of the product and the manufacturing process supported by appropriate process controls. Quality by design principles that have been established for the development of drug products/substances can equally be applied to the development of analytical procedures. This paper presents the development and validation of a quantitative method to predict the concentration of piroxicam in Kollidon® VA 64 during hot melt extrusion using analytical quality by design principles. An analytical target profile was established for the piroxicam content and a novel in-line analytical procedure was developed using predictive models based on UV-Vis absorbance spectra collected during hot melt extrusion. Risks that impact the ability of the analytical procedure to measure piroxicam consistently were assessed using failure mode and effect analysis. The critical analytical attributes measured were colour (L* lightness, b* yellow to blue colour parameters—in-process critical quality attributes) that are linked to the ability to measure the API content and transmittance. The method validation was based on the accuracy profile strategy and ICH Q2(R1) validation criteria. The accuracy profile obtained with two validation sets showed that the 95% β-expectation tolerance limits for all piroxicam concentration levels analysed were within the combined trueness and precision acceptance limits set at ±5%. The method robustness was tested by evaluating the effects of screw speed (150–250 rpm) and feed rate (5–9 g/min) on piroxicam content around 15% w/w. In-line UV-Vis spectroscopy was shown to be a robust and practical PAT tool for monitoring the piroxicam content, a critical quality attribute in a pharmaceutical HME process.

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Development of an analytical method for crystalline content determination in amorphous solid dispersions produced by hot-melt extrusion using transmission Raman spectroscopy: A feasibility study

Cited by 28 publications

References 32 publications

Quantifying low levels (<0.5% w/w) of warfarin sodium salts in oral solid dose forms using Transmission Raman spectroscopy

Quantifying low levels (<0.5% w/w) of warfarin sodium salts in oral solid dose forms using Transmission Raman spectroscopy

Multivariate Calibration for the Development of Vibrational Spectroscopic Methods

Development and Validation of an in-line API Quantification Method Using AQbD Principles Based on UV-Vis Spectroscopy to Monitor and Optimise Continuous Hot Melt Extrusion Process

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