Clinical Supplies

• Release testing
• Stability testing
• Comparator studies
• Method development and method validation
• DEA schedule I-V licenses
• Post package ID

Finished Products

• Release testing
• Stability testing
• DEA schedule I-V licenses
  

Isolations

(To see our process flow click here)

• Preparative chromatography
• Isolations
• Structure elucidation
• Purity assignment

Purification of Actives

• Preparative chromatography
• Isolations
• Purity assignment

Comparator Studies

• Method development and method validation
• Release testing
• Stability storage and testing
• Dissolution and assay method
• DEA schedule I-V licenses
• For compendial and propriety products
• Reference Standards
• Product Experience (click this link to visit our case studies)

Extractables and Leachables

• Both organic and inorganic (click here to view actual case studies)
• Develop HPLC, GC, and ICP methods for controlled extractables from pharmaceutical containers/closures/devices
• Identify extractables using GC/MS and LC/MS – obtain a profile
• Modify appropriate controlled extractable methods for use in routine extractable testing
• Validate the routine extractable methods for product release
• Modify appropriate controlled extractable methods for use in leachables testing
• Obtain a leachables profile
• Validate the leachables method for incorporation into a stability program

 

Complete Characterization

• Identification  (CHN, X, O, IR, UV/Vis, NMR(H1& C13), MS)
  
• Physical  (Melting/Boiling Point, Optical Rotation, TGA, pH)
  
• Purity  (HPLC, Residual Solvents, Titration, KF, Metals Screen, ROI)
  

RSM Program QTI performs the following services to provide a complete solution for corporate RSMs

• Initial Characterization
  
• Generation of a Certificate of Analysis
  
• Expiry Dating through stability testing
  
• Repository & Distributor
  
• Periodic Re-qualification
  
  • Complete Characterization of Sample Limited RSM
• Especially designed for impurities, metabolites, or other expensive materials
  
• Typical characterization methods requires 1 – 2 grams of material for complete characterization
  
• Sample Limited RSM characterization methods requires 100 – 200 milligrams of material for complete characterization

 

• Excipient Testing
  • Compendial Analysis (USP, EP, JP)
  • Client Specific Methodologies
• Intermediate Process Testing
• Product Release Testing

 

Current

• Method development and validation
  
• Product characterization
  
• Analysis of trace contaminants
  
• UV-Vis, RI, or fluorescence detection
  
• Light Scattering (ELSD)
  
• Chromatographic modes available:  normal and reversed phase, Ion exchange, size exclusion, semi-preparative
  
• Low Temperature Storage (0°, -20°, -40°, -80° C)
  
• Solid Phase Extraction (SPE) techniques
  
• Custom assay development
  
• High-sensitivity assays
  
• High-yield extraction processes, SPE and column based purification
  
• Early phase development, API and finished product monitoring

 

Cleaning Procedures to be followed by:

• Manufactures and contract manufactures of APIs, finished products and excipients
  
• Packagers and contract packagers

Sampling Techniques:

• Swabbing
  
• Rinsing
  
• Any other reasonable techniques

Setting Acceptable Residue Limits (ARL):

• Very important in cleaning validation; should be logically based
  
• Must be practical, achievable, verifiable
  
• Decomposition products should be checked
  
• First criteria - visually clean
  
• 10 ppm limit – pharmacopoeias limit test, assuming residues to be as harmful as heavy metal; useful for materials for which no toxicological studies are available; not for pharmacologically potent materials.
  
• NMT 0.1% of therapeutic dose limit – minimum daily dose of current product carried over into maximum daily dose of subsequent product; identify the worst case

Analytical Methods:

• Develop and validate analytical methods for cleaning validation
  
• Critical aspects to be considered- LOD, LOQ, precision, linearity, selectivity, recovery-spiking, consistency of recovery
  
• Use the validated methods to perform routine analysis of cleaning validation samples

Non-specific methods:

• TOC:
  
  • Useful for detecting all carbon containing compounds that are adequately soluble in water (which includes active species, cleaning agents and excipients)
    
  • TOC methods are sensitive to ppb range and less time consuming
    
  • Cannot identify exactly what the residue material is.
    
• Determination of Residual Micro 90
  • Can be used to determine the amount of residual Micro 90 left after the completion of cleaning procedure
    
  • Use UV/Vis detection

API Specific methods:

• Develop and validate methods to specifically identify and quantitate APIs (including biopharmaceuticals) after cleaning procedure
  
• If an active drug is highly toxic, a specific method is always recommended