Pre-formulation & analytical characterization

InhaTarget Therapeutics DPI characterization consists in the evaluation of:

  • Physicochemical properties such as crystalline properties (X-ray Powder Diffraction, differential scanning calorimetry), solvent content (thermogravimetric analysis, gas chromatography), particle size distribution (laser diffraction, dynamic light scattering), charge (zeta potential), drug content or degradation (high performance liquid chromatography coupled to UV-visible or mass detectors, atomic absorption spectroscopy, UV-visible spectrophotometry, size exclusion chromatography, SDS-page);
  • Aerodynamic performance through a dry powder inhaler such as the uniformity of delivered doses and the determination of the fine particle dose, which is the dose of drug theoretically able to be deposited into the lung (aerodynamic diameter below 5 µm) using tests recommended by European Pharmacopeia and using full resolution impactors (multi-stage liquid impactor, next generation impactor);
  • In vitro dissolution/release profiles using technique adapted for inhaled products which is recommended by ‘the Dissolution Working Group of International Pharmaceutical Aerosol Consortium on Regulation and Science’.

Facilities and equipment - physical, chemical, thermal and pre-formulation characterization

  • Modulated differential scanning calorimetry (MDSC) and thermogravimetric analysis (TGA) (MDSC Q2000, TGA.Q500 Hig Res, TA Instruments)
  • Hot Stage Microscopy (HSM) (Linkam THMS 600) and image analysis by optical microscope (Olympus BX60) assisted by camera (JVC TKC 1381) and analysis image software (Olympus AnalySis 5.1)
  • Powder X-Ray Diffraction (PXRD)*with computerized identification
  • Measurement of Solubility and intrinsic dissolution rate
  • Shape, Morphology, Size analysis: Optical microscopy, Scanning Electron Microscopy (SEM*) and Transmission electron Microscopy (TEM*)
  • Particle size and size distribution analysis: Laser diffraction, 0.02 – 2000 µm with dry and wet sampling (Malvern Mastersizer 3000) and for aerosol (Malvern Spraytec)
  • Particle size distribution for submicron analysis by Photon Correlation Spectroscopy (PCS), 2 – 3000 nm (Malvern Zetasizer Nano ZS)
  • Zeta potential determination (Malvern Zetasizer Nano ZS)
  • Combined SEM – XR mapping (JSM-6100 Scanning Electron Microscope, EDAX)*
  • Diode-array UV spectrophotometer (Agilent 8458)
  • Fourier Transform Infrared Spectroscopy (FTIR)
  • Solid state characterization
  • Viscosity determination for liquid and semi-solid formulations (Brookfield, LV-DV-II +)
  • Determination of powder flowability using tap density tester (Stampfvolumeter STAV 2003, Jel, Germany)
  • Surface area determination using BET gas adsorption*
  • Analytical systems: High-Performance Liquid Chromatography (HPLC) (Agilent 1100, 1200) with different detectors (UV-Vis, UV (VWD, DAD), mass spectrometry (LC/MS, MS/MS), refractive index (RI); Gel Permeation Chromatograpy (GPC) and Gas Chromatography (GC)
  • Mass spectrometry*: pharmacokinetic, metabolomics and proteomic: LC/MS single quad, LC/MS/MS QTOF, LC/MS/MS QQQ, NanoESI QTOF (Agilent)
  • Stability tests in climatic chambers following ICH norms (Pharma 600)
  • *see ‘Our Partners’
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