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PLS Regression Model Comparison of 60 and 300 MHz 1H qNMR of EPA and DHA
Omega-3 Fatty Acids Obtained at Different Points ...
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 On...
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-...
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 conce...
Experimental
Varian Mercury - 300 MHz NMR Supercon Spectrometer
4 pulse on pure sample in 5 mm tube, Run Unlocked
In MNova...
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...
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....
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-F...
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 Annua...
John Edwards   ACS NERM 2013 - Fish Oil Analysis -10-22-13
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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Transcript of "John Edwards ACS NERM 2013 - Fish Oil Analysis -10-22-13"

  1. 1. 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
  2. 2. 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
  3. 3. 60 MHz Reaction Monitoring
  4. 4. On-Line Process NMR 45 Systems Installed Since 1996 Predominantly in Petroleum and Petrochemical
  5. 5. 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
  6. 6. b g b a www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  7. 7. 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
  8. 8. 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
  9. 9. DHA EPA EPA EPA EPA Comparison of High EPA and High DHA PUFA-Ester after Separation
  10. 10. 300 MHz 1H NMR Spectra of Samples at Diferent Points in the Process
  11. 11. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  12. 12. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  13. 13. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  14. 14. 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
  15. 15. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  16. 16. 300 MHz 1H NMR Data Stacked and integrated. Integrals Utilized in PLS Regression Against EPA/DHA content by GC
  17. 17. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  18. 18. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  19. 19. 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
  20. 20. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  21. 21. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  22. 22. 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
  23. 23. www.process-nmr.com www.nmrblog.com Tel: 203-744-5905
  24. 24. 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
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