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John Edwards MNova User Meeting - SMASH - 9-22-13

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John Edwards MNova User Meeting - SMASH - 9-22-13

  1. 1. Process NMR Associates Utilization of MNova in a Commercial NMR Testing Laboratory for : 1) Development of Automated Quantitative Analysis Methods by Direct Internal Standard NMR Measurements, and 2) Pre-Processing of Large NMR Datasets for Chemometric Regression Analyses to Derive Chemical and Physical Properties John Edwards Process NMR Associates, LLC, Danbury, Connecticut September 22, 2013 MestreLab MNova Users Meeting, SMASH 2013 Santiago de Compostela, Spain
  2. 2. Process NMR Associates 250+ Analytical NMR Customers TTC Labs, Inc. Process Engineering Excellence Analytical Services And Consulting TopNIR Systems
  3. 3. Process NMR Associates Quantitative 1H qNMR Method for Complex Mixture Analysis: Determination of Acetylated Polysaccharides, Glucose, Maltodextrin, Isocitrate, Malic Acid in Aloe Vera Leaf Juice. Also … Preservatives, Additives, and Degradation Products in Aloe Vera Raw Materials and Consumer Products Presented By John Edwards, Ph.D. Process NMR As sociates, LLC Danbury, Connecticut November 9, 2012 Aloe Summit, Las Vegas, NV Development of Automated Quantitative Analysis Methods by Direct Internal Standard NMR Measurements
  4. 4. Process NMR Associates NMR Systems and Experimental Conditions Acquisition Time Relaxation (Recycle) Delay Frequency, MHz Nucleus Number of Pulse Accumulations* Original FID Points Zero-filled Points Pulse sequence Solvent Sweep width, ppm Temperature Line Broadening Steady State Pulses Pre-Acquisition Delay 3-8 Seconds 2-6 Seconds 300-500 MHz 1H 16-256 16384-84000 32768-262144 Single pulse D2O 16 Ambient (25 ºC) 0.35 Hz 8 60 seconds
  5. 5. Process NMR Associates Advantages of Using NMR in Complex Mixture Analysis • Minimal Sample Preparation • Reproducible (site to site, country to country) • Linear and Quantitative Spectral Response • Targeted AND Non-Targeted • Qualitative • Quantitative • Compound Specific • Rapid – 10 Minutes • Affordable
  6. 6. Process NMR Associates Aloe Vera Inner Leaf Juice Constituents and Additives that need to be Analyzed and Reported for IASC Certification Compound Acemannan Acetylated PS Glucose IASC Certification requirement ≥ 5% dry weight Present Aloin 10 ppm or less in 0.5% aloe vera solids solution, analysed by HPLC or other fit for purpose methodology approved by IASC Isocitrate ≤ 5% dry weight Maltodextrin Must be listed on label and analysis must meet label claims. If undeclared, is considered an adulterant. Solids Ash ≥ 0.46% in single-strength juice (for example, a 10x concentrate should have ≥ 4.6%) ≤ 40%
  7. 7. # # Chemical Characterization of the Immunomodulating Polysaccharide of Aloe Vera L., W.J.Goux, et al, http://www.iasc.org/AloeStructure080604.pdf
  8. 8. Process NMR Associates x y w w d c m z a m b
  9. 9. Commercial freeze-dried 200x aloe vera leaf juice powder Process NMR Associates
  10. 10. Process NMR Associates Chemical shift values, peak and chemistry descriptions, molar conversion factors that can be used for detection and quantitation of aloe vera leaf juice preservatives, additives, and degradation products Compound Type of compound Signal type Propylene glycol Ethanol Lactic acid Potassium sorbate Additive Degradation product or additive Degradation product Preservative CH3, doublet (N=3) CH3, triplet (N=3) CH3, doublet (N=3) CH3, doublet (N=3) Chemical shift, ppm 1.1 1.15 1.33 1.82 Acetic acid Pyruvic acid Citric acid CH3, singlet (N=3) CH3, singlet (N=3) 2 x CH2, Multiplet (N=4) 1.96 2.35 2.5-3.0 Succinic acid Glycerol Glycine Sucrose Fumaric acid Sodium benzoate Degradation product Degradation product Naturally present or added as pH regulator or preservative Degradation product Additive Additive Additive Degradation product Preservative 2 x CH2, singlet (N=4) CH2 and CH, multiplet CH2, singlet (N=2) CH, doublet (N=1) 2 x CH, singlet (N=2) 2 x CH, doublet (N=2) 2.6 3.5 3.51 5.4 6.5 7.95 Formic acid Degradation product CH, singlet (N=1) 8.2-8.3
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  18. 18. Process NMR Associates 2) Pre-Processing of Large NMR Datasets for Chemometric Regression Analyses to Derive Chemical and Physical Properties
  19. 19. Process NMR Associates Third Generation NMR - 2013– Aspect AI NMR System New magnet design – 30mm bore size • The amount of magnetic pieces that assemble the magnet reduced from 34 to 10. Reduction in Mechanical Complexity • Bore size of the magnet was increased to 30 mm - improved temperature susceptibility • Improved temperature and shim stability. New Digital Spectrometer Design - reduces footprint, improves signal processing capabilities Probe - Improved Probe Q for Higher Sensitivity. Software – Windows 7 – Improved Chemometric Capabilities Lab version On-Line version
  20. 20. Process NMR Associates Pulsar 60 MHz NMR 3-5 mm Samples Lab Only 42 MHz NMR 3-5 mm Samples Lab Only NMReady 60 60 MHz NMR 3-5 mm Samples Lab Only September 12, 2013 Fourier 60 MobiLab™ SPECTRA 2T 60 MHz NMR 3-5 mm Samples Lab Only 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 aspectimaging 60 MHz NMR 3-10 mm Samples Lab or On-Line 60 MHz NMR 3-10 mm Samples Lab or On-Line
  21. 21. Process NMR Associates NMR Data Processing for Input into Chemometrics – PCA/PLS
  22. 22. 1H NMR Reaction Monitoring – Esterification of t-butanol with acetic anhydride
  23. 23. CH3 O HO + H3C A CH3 H3C H3C O O CH3 O CH3 B H+ D + O H3C O CH3 OH E H3C C A B D C E Acid Catalyzed Esterification of Iso-Butanol with Acetic Anhydride
  24. 24. T-BuOH T-Bu-Ester Esterification of t-BuOH Ac-Ester Integral Graph Acetic Acid And Integration Plot AcAn 2.5 2.0 1.5 1.0 ppm
  25. 25. 1H NMR – Sucrose Hydrolysis by Invertase Enzyme Sucrose a-glucose
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  30. 30. Process NMR Associates Transposed CSV Output of Stacked Plot – Yields rows that have integration bin values Input as X Variable Data into Chemometrics Software Packages
  31. 31. PLS Regression Analysis to Obtain Predictive Model of EPA and DHA Omega-3 Fatty Acids at Various Points Of Nutritional Supplement Manufacturing Process EPA (Area %) 0.64 21.55 62.97 29.43 14.21 52.74 15.21 7.18 16.95 36.35 61.09 13.32 71.78 41.40 1.19 11.73 43.38 6.07 9.77 58.93 10.62 43.91 54.05 0.00 26.97 DHA (Area %) 0.01 13.34 15.66 18.16 9.54 28.90 10.51 0.23 10.04 16.47 21.26 5.95 7.43 25.91 0.06 12.23 19.30 2.78 0.72 23.41 5.18 21.52 28.18 0.00 12.82 Sample Description First Esterification First Esterification Clathration Mol Dist Pollock Oil Separator PolyUnsat Ester First Esterification First Esterification Clathration Mol Dist MSC Pollock Oil Separator PolyUnsat Ester First Esterification First Esterification Clathration Clath Raffinate First Esterification Mol Dist MSC Pollock Oil Separator PolyUnsat Ester First Esterification First Esterification 600 500 400 300 Data NMR ID FO3h001 FO3h002 FO3h003 FO3h004 FO3h005 FO3h006 FO3h007 FO3h008 FO3h009 FO3h010 FO3h011 FO3h012 FO3h013 FO3h014 FO3h015 FO3h016 FO3h017 FO3h018 FO3h019 FO3h020 FO3h021 FO3h022 FO3h023 FO3h024 FO3h025 200 100 0 -100 1 2 3 4 5 6 Variables 7 8 9 10 11
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  36. 36. Process NMR Associates Acknowledgements Paul Giammatteo – PNA Tal Cohen – ASPECT AI and Modcon Adam Dicaprio, Daniel Edwards – PNA Mike Bernstein – MestreLabs (SMA Development) For more information and applications visit www.process-nmr.com

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