XRPD for Small‑Molecule Drugs
Comprehensive X‑ray powder diffraction analysis for pharmaceutical APIs and formulations — from polymorphism screening to batch release testing with cGMP compliance.
XRPD Throughout Drug Development
XRPD is an essential analytical technique for the characterization of small-molecule drugs, providing direct information about the solid state of an active pharmaceutical ingredient (API). XRPD patterns form a critical aspect of patent applications for new polymorphic forms.
XRPD for API Development
Since XRPD patterns are directly related to the crystalline structure of a material, this is an ideal technique for the screening, identification and characterization of polymorphic forms and new chemical entities in API discovery and development.
The XRPD pattern or crystal structure of a compound — whether hydrate or solvate — is often important in securing a patent. The technique can also be used to provide key data to support regulatory submissions and new drug applications (NDAs).
XRPD can be used to determine the crystallographic structure or identify the type and dimensions of the unit cell of crystalline pharmaceutical compounds. The most fundamental application of XRPD in drug development is in the identification and analysis of crystalline phases, such as polymorphs, hydrates and solvates.
XRPD Testing of Raw Materials
XRPD serves as an important tool for controlling purity, crystallinity and polymorphism for API and excipients.
Identity Confirmation
Verification of polymorphic form and crystalline structure against reference standards.
Purity Assessment
Detection and quantification of polymorphic impurities down to parts‑of‑percent levels.
Crystallinity Determination
Quantification of amorphous content in crystalline materials and vice versa.
XRPD for Preformulation & Formulation
The non‑destructive nature of XRPD makes it a suitable technique for systematic preformulation studies and for testing drug‑excipient compatibility. Excipient interactions are critical to the consistent release and bioavailability of the API.
Developers must be able to fully understand and control this behavior to avoid potentially costly late‑stage problems caused by formulation instability. Development scientists looking to optimize formulations and drug release rely on XRPD data to:
- Screen for the polymorphs of a compound
- Quantify polymorphic impurities
- Determine crystallinity and assess crystallite size
- Analyze actual percentages of an API in the final dosage form
- Quantify percentages of crystalline or amorphous excipients
- Detect potential solid‑state transformations during tableting processes
- Monitor transformations arising from a compound's hygroscopicity
XRPD for Manufacturing & QC During Batch Release
XRPD is used to monitor the quality of the finished drug product by determining the micro‑structural parameters of the API and by detecting and quantifying the presence of pharmaceutical polymorphic contaminations.
XRPD enables optimization of pharmaceutical process parameters and production control. It is used to assess the percentage of crystallinity and the morphology of active ingredients and fillers during manufacture.
This is important since any change in the morphology of fillers or in the crystalline state of active ingredients in the final product can influence a drug's solubility and bioavailability.
XRPD can also be used to monitor batch/dosage uniformity and to ensure final product stability.
cGMP Batch Release
GMP‑compliant QC testing at DANNALAB is offered with a turnaround time of as little as 24 hours.
QA‑approved Certificates of Analysis (CoA) issued for regulatory compliance.
Process Optimization
Monitoring of crystallinity, morphology, and polymorphic form throughout the manufacturing process.
Stability Monitoring
Detection of polymorphic transformations and degradation during storage and accelerated stability studies.
DANNALAB XRPD Capabilities
Detection & Quantification
- LOD: down to 0.17% wt for polymorphic impurities
- LOQ: as low as 0.5% wt in finished dosage forms
- Crystallinity: LOQ ~1% wt for amorphous/crystalline ratio
- Peak position accuracy: 10× better than Ph.Eur requirements
Regulatory Compliance
- USP<941> and Ph.Eur<2.9.33> compliant
- cGMP operations with QA oversight
- 21 CFR Part 11 traceable data
- QA‑approved CoA for batch release
Unit Cell ID
Indexing for unique polymorphic fingerprinting
Rietveld Analysis
Full‑pattern fitting for structure refinement
Special Samples
Cytotoxics, air‑sensitive, microquantities (0.002g)
Fast Turnaround
24-48h available for urgent projects
Related Services
XRPD Method Information
Detailed technical information about our XRPD methods and capabilities.
Pharmaceutical Patents
Analysis and comparison of XRPD patterns vs. patent specifications to avoid infringement.
cGMP Compliance
Full details on our quality system, certifications, and regulatory compliance.
XRPD for Stability Studies
XRPD is a critical tool for monitoring solid-state stability of pharmaceutical products during accelerated and long-term stability studies. Polymorphic transformations, hydrate formation, amorphous-to-crystalline conversion, and degradation can be detected and quantified.
Polymorphic Stability
Monitor transformations between polymorphic forms during storage. Detect unwanted phase changes affecting dissolution, bioavailability, and shelf life.
Hydrate Formation
Identify and quantify hydrate formation in hygroscopic APIs. Critical for products sensitive to moisture exposure during storage.
Amorphous Stability
Quantify crystallization in amorphous solid dispersions (ASDs). Early detection of recrystallization before product performance is compromised.
Primary Packaging Effects
Comparative studies of different blister types (PVC, PVC/PVDC, Alu/Alu) assessing moisture protection and impact on polymorphic stability.