John Edwards   ACS NERM 2013 - Fish Oil Analysis -10-22-13
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John Edwards ACS NERM 2013 - Fish Oil Analysis -10-22-13

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John Edwards   ACS NERM 2013 - Fish Oil Analysis -10-22-13 John Edwards ACS NERM 2013 - Fish Oil Analysis -10-22-13 Presentation Transcript

  • PLS Regression Model Comparison of 60 and 300 MHz 1H qNMR of EPA and DHA Omega-3 Fatty Acids Obtained at Different Points in a Fish Oil Nutritional Supplement Manufacturing Process John C. Edwards and Paul J. Giammatteo Process NMR Associates, LLC, 87A Sand Pit Rd, Danbury, CT 06810 USA Presented at the ACS North-East Regional Meeting October 23, 2013 New Haven, CT www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • Pulsar 42 MHz NMR 3-5 mm Samples Lab Only 60 MHz NMR 3-5 mm Samples Lab Only NMReady 60 60 MHz NMR 3-5 mm Samples Lab Only 60 MHz NMR 3-10 mm Samples Lab or On-Line MobiLab™ SPECTRA 2T Fourier 60 60 MHz NMR 3-5 mm Samples Lab Only Cryogen Free Permanent Magnet High Resolution Benchtop NMR aspectimaging 60 MHz NMR 3-10 mm Samples Lab or On-Line 85+ MHz NMR 3-5 mm Samples Lab Only Picospin 45 and 80 45 MHz and 82 MHz NMR 300 micron capillary injection Lab Only 60 and 90 MHz 5 mm Samples Lab Only
  • 60 MHz Reaction Monitoring
  • On-Line Process NMR 45 Systems Installed Since 1996 Predominantly in Petroleum and Petrochemical
  • 2 x Varian Mercury 300 Liquids 1 x Varian UnityPlus-200 Solids Multiple 10/20/40 mm TD-NMR 20-25 MHz NMR MOUSE 2 x Aspect-AI 60 MHz HiRes-NMR 3 x Qualion 60 MHz HiRes NMR MicroESR Shimazu GC MNova(Verify, qNMR, DB), ACDLabs Chemometrics: GramsIQ, Eigenvector Solo, Pirouette
  • b g b a www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • 50 sample initial data set from all points in manufacturing process. First round of PLS regression analysis revealed concentration outliers that were linked to limitations in the GC method. This study was performed on improved GC data values. Final 80 Sample models were utilized to validate the calibrations on a 24 sample validation set
  • Experimental Varian Mercury - 300 MHz NMR Supercon Spectrometer 4 pulse on pure sample in 5 mm tube, Run Unlocked In MNova 8.1.2 SPC Files Imported, Stacked, Binned at 3 Hz interval, Area Normalized to 100, Saved as Transposed Ascii Matrix PLS Regression Performed Thermo Grams IQ and Eigenvector Solo 300 MHz 1H NMR In chain CH2 Ethyl CH3 EPA w3 CH3 DHA Olefins CH3-CH2-O-OC-CH2-R =C-CH2-C= EtOOC-CH2-R R-CH2-C= EPA DHA w6/ w9 CH3
  • DHA EPA EPA EPA EPA Comparison of High EPA and High DHA PUFA-Ester after Separation
  • 300 MHz 1H NMR Spectra of Samples at Diferent Points in the Process
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • Samples/Scores Plot of SPC Files in MNova.xlsx First Esterification Clathration Molecular Distillate Pollock Oil Separator Product PUFA Ester Clathration Raffinate MUFA Ester Salmon Oil 95% Confidence Level 15 Scores on LV 2 (0.64%) 10 5 0 -5 -10 -15 -20 -200 -150 -100 -50 0 50 Scores on LV 1 (98.04%) 100 150 200 www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • 300 MHz 1H NMR Data Stacked and integrated. Integrals Utilized in PLS Regression Against EPA/DHA content by GC
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • Fusion of 1H NMR and FTIR-ATR Spectra – absolute intensity scaling FTIR-ATR Spectra NMR Spectra www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • Regression Results for Various NMR Approaches PLS Regression Data 60 MHz NMR 300 MHz NMR Peak Integral Data Fused - NMR-FTIR EPA Content (Wt%) DHA Content (Wt%) R2, SECV (Wt%) R2, SECV (Wt%) 0.988, 1.68 0.991, 1.09 0.993, 2.13 0.992, 1.13 0.981, 2.71 0.964, 2.24 0.993, 1.62 0.992, 1.08 www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  • Acknowledgements Daniel Edwards Generic Customer Aspect AI – NMR Systems Cosa-Xentaur Think About Attending the 2nd Annual Practical Applications of NMR in Industry Conference February 3-5, 2014 Charlotte, NC Agenda and Registration Information can be found at: http://www.panicnmr.com/ www.process-nmr.com www.nmrblog.com Tel: 203-744-5905