Dataset related to amorphous solid dispersions composed of a poorly soluble drug - bosentan & copovidone

Published: 21 February 2023| Version 1 | DOI: 10.17632/t8z4nhv2j7.1


This repository provides raw data related to : 1. Intrinsic dissolution studies of bosentan from binary solid dispersions prepared using nano spray drying and high energy ball milling. 2. 1H NMR spectra of bosentan, copovidone, and binary formulations recorded in DMSO-d6 and CDCl3. 3. ATR-IR spectra of binary formulations. 4. Raw data of DSC & TG scans of nano spray dried formulation loaded with 20% (wt.) of bosentan and 80% (wt.) of copovidone. Description of Methods Intrinsic dissolution studies The binary formulations (100 mg of powder, 8 mm in diameter) were compacted in disc holders using Atlas™ manual 15 t hydraulic press (Specac, Kent, UK) with a load pressure of 2 t applied to each sample for 30 s. Then disc holders with compacts were mounted on rotating shafts (100 rpm). The test was performed at 37 °C using 500 mL of 1 % sodium lauryl sulfate as a solvent. The concentration of bosentan dissolved was determined spectrophotometrically (Shimadzu UV-1800, λ = 264 nm). 1H NMR measurements The spectra were recorded at 21 °C using a FT-NMR 500 MHz (JNM-ECZR500 RS1 v. ECZR, JEOL, Japan) spectrometer with Delta software. Ten milligrams of the sample were dissolved in 0.75 mL of deuterated dimethyl sulfoxide (DMSO-d6, Chemat, Gdańsk, Poland) or chloroform (CDCl3, Chemat, Gdańsk, Poland). These solutions were placed in 5-mm diameter NMR tubes and spectra were recorded. Raw data was exported into ASCII files (*1HNMR*.asc). The details on the protocol used for 1H NMR measurements were described in files (*.hdr). Attenuated total reflectance - Infrared spectroscopic (ATR-IR) studies These measurements were carried on a Nicolet iS5 spectrometer (Thermo Scientific) equipped with an iD3 ATR with ZnSe crystal window in the range of 4000-525 cm-1 with a resolution of 2 cm-1 and a total of 64 scans. The atmospheric interference (CO2, H2O) has been automatically subtracted using dedicated Thermo Scientific™ OMNIC™ software. Differential scanning calorimetry (DSC) analyses The measurements were carried out using a Mettler Toledo DSC 3+ differential scanning calorimeter (Switzerland) with the software STARe v.16.4 (5 °C/min, Ar 5.0). Thermogravimetric analyses (TG) Mettler Toledo TGA/SDTA 851e apparatus was used. The measurements were carried out in Ar 5.0 (50 mL/min) at the temperature range from 25 °C up to 300 °C at the constant heating rate of 5 °C/min.



Uniwersytet Jagiellonski w Krakowie


Drug Development, Nuclear Magnetic Resonance Spectroscopy, Differential Scanning Calorimetry, Amorphous Alloy, Dissolution, Solid Phase Dispersion, Pharmaceutics, Drug Solubility, Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy


Narodowe Centrum Nauki