Analytical techniques

XRPD is the main technique for characterization of pharmaceutical solids. XRPD is used for formulation control, crystallinity or amorphous content measurements, desolvation or polymorphic transition monitoring, or raw material control.
Holodiag owns two very versatile and high-performance systems that cover most of the analytical needs.
Their different setups allow to provide specific answers for a given problem on a wide range of samples:

• Low API concentrations
• Wet powder
• Slurries or suspensions
• Tablets or pills
• Very low quantities, etc.
The integrated sample changers procure high-throughput capability to the systems.
Moreover, XRPD enables high scan rate analyses for the observation of fast phase transitions (polymorphism, desolvation, …).
Results can be correlated to additional thermal techniques we have available in-house, like DSC or TGA.
Our team can carry out the analyses under controlled atmosphere and conduct preparation of air-sensitive samples.

Holodiag owns two Dynamic Vapor Sorption devices.
Our systems, a DVS Intrinsic (SMS), allow to monitor sample mass variation vs. Relative Humidity.
This enables accurate depiction of hydrate stoichiometry and stability, hygroscopicity and drying conditions.

Holodiag owns a spectrometer to quickly and accurately perform infrared spectra.
The Attenuated Total Reflectance (ATR) system with diamond window allows to easily analyze powders and liquids.
Specific investigations such as API/excipients compatibility can be carried out by infrared (IR) spectroscopy.

Holodiag owns a high precision thermo-gravimetric analyzer. Results can easily be correlated to complementary calorimetric or structural analyses.
Thermo-gravimetric analysis allows to follow weight losses of a sample as a function of temperature.
It is used in numerous applications:
• Desolvation / dehydration
• Stability control (solvates/hydrates)
• Degradation
• Loss on drying
• Quantification, etc.
The integrated sample changer gives high throughput capabilities.

Holodiag owns a high precision Differential Scanning Calorimeter.
Differential scanning analysis allows the characterization of thermal events as a function of temperature.
It is used in numerous applications :
• Polymorphic transitions
• Melting / degradation
• Thermal stability (e.g. additive effects)
• Security testing
• Amorphous content
• Glass transition
• Characterization of desolvation
• Quantification, etc.
The variety of available sample pans allows to design a large diversity of analyses. Samples can be prepared in a glove box under inert gas to avoid any degradation or transformation before analysis.
The integrated sample changer gives high throughput capabilities.

Our UV spectrometer can perform UV-visible spectra and accurately measure absorbance values. Its main applications are the determination of λmax and solution concentration monitoring.

Holodiag owns an automatic volumetric titration system. The Karl Fischer method allows for accurate water titration by specific oxydo-reductive reaction. A typical application is the determination of hydrate stoichiometry.

Holodiag owns a Mastersizer 3000 granulometer (dry and liquid mode) fully set and qualified inside a laminar flow hood for toxic samples handling.
We propose analytical method development and validation, QC and routine analyses.

Holodiag is equipped to perform density and flowability measurements according to Ph. Eur 2.9.34.
We propose bulk/tapped density with Hausner ratio in order to evaluate the flow behavior of powder.

Holodiag performs Intrinsic Dissolution Rate measurements according to Pharmacopoeia using Dissolutest Vision G2 Elite 8.
As integral part of API solid form characterization, it is key data for relevant form selection and solid state dissolution comparisons.