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Analytical & Bioanalytical Techniques

Analytical & Bioanalytical Techniques. Joshua Hicks Catalent Pharma Solutions September 2, 2015. NMR quantification vs. other methods. NMR. For automated, internal-standard-free, absolute quantization… NMR is accurate, precise and versatile Superior to CLND ELSD Weighing. CLND. ELSD.

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Analytical & Bioanalytical Techniques

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  1. Analytical & Bioanalytical Techniques Joshua Hicks Catalent Pharma Solutions September 2, 2015

  2. NMR quantification vs. other methods NMR • For automated, internal-standard-free, absolute quantization… • NMR is accurate, precise and versatile • Superior to • CLND • ELSD • Weighing CLND ELSD • Analytical Chemistry (2005), 77(14), 4354-4365

  3. Quantificaiton with Internal Standard (IS) • X mg of Compound • X mg of IS • Purity of IS Concentration of Compound? Purity of Compound?

  4. Using PULCON J Am Chem Soc. 2006 Mar 1;128(8):2571-6. Reference Standard for PULCON NMR of Sample Calibrated to a sample of known concentration, known number of protons 10 mM & P1 Calibration NS TE Integrals # Protons P1 Calibration NS TE Integrals # Protons Concentration of Unknown

  5. Accuracy of Analysis? • Considerations for Reducing Error in Quantification • Sample Prep • Parameter Set • Field Strength (less error at higher fields) • Probe • Instrument stability • Method of integration (Region or Linefit) • Room stability • SOPs • Calibrant Region (pure) Linefit (overlap)

  6. A Tale of Two Probes Single sample, same instrument – does configuration matter?

  7. Quantification of Compounds in Crude Extract * * * * 32.8mM

  8. Youden Ruggedness’ Trial • 600 MHz vs. 400 MHz • NMR Tube Quality • Different concentration • Different gravimetric balance • Different pulse sequence • Different days Mesh Size (Also EtOH:Leaf) Chlorogenic Acid BBE Delta ~ 2% 600 400 7

  9. Benefits of High Quality Data: L-Carvone Red = double presat Blue = Wetdc L-Carvone Water DMSO 100 Hz

  10. QC/QA System • Non-NMR user • Simple interface • Lockdown • Automated • Suitability test • Acqu/Proc • Identification • Quantification • Report

  11. Towards Automatic Analysis • Quantification • Proton, fluorine, and phosphorus • Identification of residual solvents • Assist with identification of ‘unknown’ signals • System: • PDF report • Concentration verification (based on spectra and submitted compound) • Verification by either: • Proton only • Or proton+carbon • Or proton+hsqc • Stop light evaluation of atom assignment

  12. discover more. CATALENT PHARMA SOLUTIONS14 SCHOOLHOUSE ROADSOMERSET, NJ 08873 + 1 866 720 3148 www.catalent.com

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