Evidence map›Paper›PMID 40244320›Full record

ArticleAAPS PharmSciTech2025

The Amorphous State of the Antiepileptic Clobazam: Preparation and Characterization.

Marina M Marcos Valdez, Julio Sanchez, María E Bertotto, Octavio E Fandiño, Fernando P Cometto, Norma R Sperandeo

Abstract read
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In one paragraph

Article in AAPS PharmSciTech, 2025. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 1 paper.

0numbers the graph read from it
0cells of the map it votes in
1citing papers in PubMed
–field-weighted citation impact
1 · What the graph read from it

What it found

Each row is one number read from the abstract, on the scale the paper reported it, with its interval. Left of the dashed line favours the treatment, right favours the comparator. Under each row is the sentence it came from. New to these charts? A ten-minute tutorial.

The abstract states no effect estimate the extractor could read, or names no intervention and outcome on the map, so this paper lights no cell and moves no belief. It is still indexed, cited and linked below.

2 · The registry

The trial behind it

Trials whose registry record cites this paper, or whose number appears in the abstract. A trial that started after this paper was published is citing it as background, not reporting it.

Neither the registry nor the abstract names a trial number. If this is a trial report, that itself is worth knowing.

3 · Its place in the literature

Who cites it

1 citing paper in PubMed.

  1. Article
4 · The record

Corrections and comments

PubMed lists nothing against this paper. Absence here is not a guarantee, only a check that was made.

5 · Who and what money

Authors and funding

6 authors.

Marina M Marcos ValdezFacultad de Ciencias Químicas, Departamento de Ciencias Farmacéuticas y Unidad de Investigación y Desarrollo en Tecnología Farmacéutica (UNITEFA)-Consejo Nacional de Investigaciones Científicas y Técnicas de la República Argentina (CONICET), Universidad Nacional de Córdoba, Ciudad Universitaria, Córdoba, X5000HUA, Argentina.
Julio SanchezDepartamento de Materiales Centro, INTI-Dirección Técnica Centro Occidental-Regional Córdoba, Av. Vélez Sarsfield 1561, Córdoba, X5000 JKC, Argentina.
María E BertottoFacultad de Ciencias Químicas, Departamento de Ciencias Farmacéuticas, Universidad Nacional de Córdoba, Ciudad Universitaria, Córdoba, X5000HUA, Argentina.
Octavio E FandiñoFacultad de Ciencias Químicas, Departamento de Ciencias Farmacéuticas y Unidad de Investigación y Desarrollo en Tecnología Farmacéutica (UNITEFA)-Consejo Nacional de Investigaciones Científicas y Técnicas de la República Argentina (CONICET), Universidad Nacional de Córdoba, Ciudad Universitaria, Córdoba, X5000HUA, Argentina.
Fernando P ComettoDepartamento de Fisicoquímica, Facultad de Ciencias Químicas, Universidad Nacional de Córdoba, Ciudad Universitaria, Córdoba, X5000HUA, Argentina.
Norma R SperandeoFacultad de Ciencias Químicas, Departamento de Ciencias Farmacéuticas y Unidad de Investigación y Desarrollo en Tecnología Farmacéutica (UNITEFA)-Consejo Nacional de Investigaciones Científicas y Técnicas de la República Argentina (CONICET), Universidad Nacional de Córdoba, Ciudad Universitaria, Córdoba, X5000HUA, Argentina. norma.sperandeo@unc.edu.ar.ORCID http://orcid.org/0000-0002-2380-6328

Funding

Secretaria de Ciencia y Tecnología - Universidad Nacional de Córdoba PID CONSOLIDAR. Res. N° 411/18.
6 · The paper itself

Abstract

The aim of this study was to prepare and characterize amorphous clobazam (CLOB) and investigate its devitrification under various stressors (temperature/humidity, compaction and mechanical/thermal stresses). Amorphous CLOB was prepared by melt-quenching in liquid nitrogen. The quench-cooled sample (CLOB-q) was characterized via polarized light and hot-stage microscopies (PLM and HSM), X-ray powder diffraction (XRPD), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), conventional and modulated DSC (DSC-c and MDSC®), thermogravimetry (TG), dynamic mechanical analysis (DMA), X-ray photoelectron spectroscopy (XPS) and contact angle measurements. Stability of CLOB-q toward temperature/humidity, compaction, and combined mechanical and thermal stress were also evaluated. CLOB-q was a truly amorphous form, as revealed by DSC-c, MDSC® and DMA. Its calorimetric glass transition temperature (Tg) was 67.0 °C (20 °C/min) and the ratio Tm/Tg was 1.34, indicating a fragile glass. The water contact angle of CLOB-q (121.8° ± 1.7°) was lower than that of crystalline CLOB (CLOB-c, 131.3° ± 3.6°), likely due to its higher concentration of surface CL, as determined by XPS. Storage of CLOB-q at - 20 °C/0% RH, 25 °C/0% RH and 40 °C/75% RH resulted in its complete devitrification to CLOB-c within 60 days, 4 days, and 42 h respectively. Subjection of CLOB-q to compaction (19.6 kN) and combined mechanical-thermal stresses also resulted in complete crystallization to CLOB-c. In conclusion, amorphous CLOB was successfully prepared in the laboratory for the first time and thoroughly characterized. It easily devitrified to CLOB-c by effect of different stressors, and thus it could not have advantages over CLOB-c in terms of physical stability.

Indexed as

AnticonvulsantsBenzodiazepinesCalorimetry, Differential ScanningChemistry, PharmaceuticalClobazamCrystallizationDrug StabilityHumidityPhotoelectron SpectroscopySpectroscopy, Fourier Transform InfraredTemperatureThermogravimetryTransition TemperatureX-Ray DiffractionAnticonvulsantsBenzodiazepinesClobazam1,5-benzodiazepinesconventional and modulated DSCdevitrificationdynamic mechanical analysisX-ray photoelectron spectroscopy

Identifiers

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Registered trials

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Read under generation 80e0d062 · epoch 390. Bibliography from PubMed, PubMed Central and OpenAlex; grants from NIH RePORTER; trial links from ClinicalTrials.gov; estimates, votes and beliefs from the OpenQuestion graph.