Organic assay & impurity testing

 

Nitrosamines, such as N-nitrosodimethylamine (NDMA) are reported to be a probable human carcinogens. A recent FDA statement revealed that NDMA impurities were found in ranitidine medicines, leading to the recall of the blood pressure and heart medications losartan, valsartan and irbesartan.

The FDA is reported to have requested that drug companies conduct laboratory testing to examine levels of NDMA and related impurities in ranitidine, as well as other drug products.

Recent guidance issued by the FDA confirms a triple quadrupole LC-MS/MS method may be used as an alternative or confirmatory method for the LC-HRMS method.

LGC have developed and validated LC-MS/MS methodology, with improved specificity, suitable for the determination of a full range of drug product and process related Nitrosamines, including NDMA and NDELA:

  • N-Nitrosodibutylamine      
  • N-Nitrosodiphenylamine      
  • N-Nitrosodi-n-propylamine       
  • N-Nitrosomethylethylamine      
  • N-Nitrosomorpholine      
  • 1-Nitrosopiperidine      
  • 1-Nitrosopyrrolidine

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Capabilities
Not only do LGC have access to the latest state-of-the art analytical equipment, we continually work with instrument manufacturers to push the boundaries of separation sciences. Our scientists combine a wealth of technical expertise with extensive knowledge of industrial and regulatory requirements to support both routine and tailored analytical testing of a broad spectrum of compounds and dosage forms to your specific needs.

Techniques

  • HPLC and UPLC with PDA, MS, UV
  • GC and Headspace GC with FID, ECD, MS (Agilent 7890B GC with Agilent 5977 MSD)
  • High resolution LC-MS
    • Waters Acquity H-Class (PDA) with Waters Synapt G2 Q-TOF MS (with Ion Mobility Separation)
    • Waters Acquity H-Class (PDA) with Waters Xevo G2 XS MS
  • Supercritical fluid chromatography (SFC) with PDA, MS
  • TLC
  • Dissolution
  • Optical Rotation
  • Titration
  • pH
  • Conductivity
  • Karl Fisher

 

Applications

  • ID, potency and purity testing of drug substance and drug product
  • Raw material, excipient and active substance testing
  • Materials testing to USP, EP, BP and JP compendial monographs
  • Full release and in-process testing
  • Phase appropriate method development, optimisation, qualification, validation and transfer
  • Impurity profiles and specification limit development including N-nitrosodimethylamine (NDMA) analysis
  • Genotoxin method development and testing
  • Solubility and dissolution studies
  • Excipient compatibility tests
  • Content and blend uniformity
  • Residual solvents and water content analysis
  • Stability Testing
    • Protocol design
    • Accelerated and long-term stability testing
    • Drug substance stability testing
    • Finished drug product stability testing (solid oral dose, inhaled and nasal, parenteral, topical/creams)
    • Comparator testing and bioequivalence studies
    • Photostability (ICH Q1B)
    • Temperature cycling studies