GMP X-Ray Powder Diffraction Pharmaceutical Analysis

GMP X-ray powder diffraction analysis can provide a wealth of information to support your drug development, regulatory submission data and GMP release testing requirements. Pharmaceutical intermediates, APIs and final products can exhibit polymorphism. Powder XRD can be used to observe polymorphic changes that may occur during storage or manufacturing. Temperature and time variations on storage can initiate changes in the original powder pattern. Pharmaceutical manufacturing processes such as grinding, physical compaction can affect the morphology of the physical forms of pharmaceutical materials such as active ingredients.

X-ray powder diffraction (XRPD) is a core technique for the identification and characterization of solid pharmaceutical materials in terms of the structural order or disorder of solid APIs or other substances. Solid forms of a given molecule exhibiting long-range crystalline order (e.g., polymorphs, solvates, co-crystals, and salts) can be identified and characterized using XRPD by their unique combination of order parameters and well defined sharp diffraction peaks. Different phases, or polymorphs, within a particular material can be distinguished from one another by their unique X-ray powder diffraction (XRPD) patterns. Comparison against a library database of expected polymorph or reference materials facilitate confirmation.

Key X-ray Powder Diffraction Expertise
Forming a key technique in our GMP physical characterization laboratory, our scientists apply XRPD to crystal morphology requirements supporting drug development, regulatory submission data and GMP lot release. We also provide GLP compliant XRD services.

Our scientists apply XRD to detect crystallographic changes in the final dosage form. This information can be used to monitor and control the quality of API’s, raw materials, excipients and finished products. By monitoring the polymorphic forms of a drug substance, it is possible to relate the data to various chemical and physical properties, including melting point, chemical reactivity, apparent solubility, dissolution rate, optical and mechanical properties vapour pressure, and density.

We also use XRPD to provide information that can assist in process development and process control, for example, studies of the impact of physical processing such as tabletting has on a specific polymorph in relation to the product’s dissolution properties. XRPD is especially valuable for analysing the percentages of individual active ingredients in the final dosage form of a drug together with the percentage of any excipients used. 

Powder XRD Services to support research, GLP or GMP requirements:

• Identification of existing forms of the active pharmaceutical ingredient (API)
• Identification of the type of order present in the API (crystalline and/or amorphous)
• Studies of physical and chemical stability
• Identification of the solid form of the API in the drug product
• Identification of excipients present in a drug product
• Detection of impurities in a drug product
• Quantitative analysis of mixtures of crystal forms

Intertek applies R&D, Good Laboratory Practice (GLP) or Good Manufacturing Practice (cGMP) compliant powder X-ray diffraction (pXRD) analysis to meet clients' physical characterization requirements. Applications include process development support, ICH stability studies, pharmaceutical quality control testing or QC batch release testing. Bringing quality and safety to life, we offer Total Quality Assurance expertise to help you to meet and exceed quality, safety and regulatory standards.