Article Figures & Data
Figures
Tables
Data Supplement
- Supplemental Data -
Supplemental Methods
Supplemental Results
Supplemental Equation S1. Number of double bond equivalents.
Supplemental Figure S1. Enhanced view of 1H NMR spectrum of solanidine showing four methyl resonances in CD3OD. Insert showing C6-H (į = 5.45, 3JH-H = 5.6 Hz, 1H) and C3-H (į = 3.40, m, 1H) resonances.
Supplemental Figure S2. 1H spectrum of SSDA
Supplemental Figure S3. Enhanced view of 1H NMR spectrum of the unknown CYP2D6 biomarker showing four methyl resonances in CD3OD. Insert showing methylylidene resonance.
Supplemental Figure S4. Stepwise connectivity model of unknown CYP2D6 biomarker. a = Ambiguous assignment of C-1, C-2 and C-24. X = C or heteroatom. Hydrogen atoms omitted for clarity.
Supplemental Figure S5. Stepwise connectivity model of unknown CYP2D6 biomarker. a = Ambiguous assignment of carbons 1, 2, 24. X = C or heteroatom. Hydrogen atoms omitted for clarity.
Supplemental Figure S6. 2D TOCSY with enhanced view of C2-H' correlations with C1-H' and/or C15-H'. Red circle represents missing C15-H correlation.
Supplemental Figure S7. 2D TOCSY with enhanced view of C1-H' and C1-H correlations C2-H' and C2-H.
Supplemental Figure S8. Stepwise connectivity model of unknown CYP2D6 biomarker. X = C or heteroatom. Hydrogen atoms omitted for clarity.
Supplemental Figure S9. Stepwise connectivity model of unknown CYP2D6 biomarker. X = C or heteroatom. Hydrogen atoms omitted for clarity.
Supplemental Figure S10. Stepwise connectivity model of unknown CYP2D6 biomarker. X = C or heteroatom; R = C or heteroatom; R’ = C or heteroatom. Hydrogen atoms omitted for clarity.
Supplemental Figure S11. Stepwise connectivity model of unknown CYP2D6 biomarker. X = heteroatom. Hydrogen atoms omitted for clarity.
Supplemental Figure S12.13C{1H} NMR spectrum of SSDA.
Supplemental Figure S13. Enhanced 13C{1H} NMR spectrum of SSDA.
Supplemental Figure S14. DEPT135 13C{1H} NMR spectrum of SSDA.
Supplemental Figure S15. DEPT90 13C{1H} NMR spectrum of SSDA.
Supplemental Figure S16. HSQC full spectrum of SSDA in CD3OD.
Supplemental Figure S17. HSQC enhanced spectrum of SSDA in CD3OD.
Supplemental Figure S18. HMBC spectrum of SSDA in CD3OD.
Supplemental Figure S19. HMBC spectrum of SSDA in CD3OD with C6íH correlations.
Supplemental Figure S20. HMBC enhanced spectrum of SSDA in CD3OD.
Supplemental Figure S21. HMBC enhanced spectrum of SSDA in CD3OD with C18íH, C19íH, C21íH and C27íH correlations.
Supplemental Figure S22. HMBC spectrum of SSDA in CD3OD with long range J filter width = 6 Hz.
Supplemental Figure S23. HMBC enhanced spectrum of SSDA in CD3OD with long range J filter width = 6 Hz.
Supplemental Figure S24. HMBC spectrum of SSDA in CD3OD with long range J filter width = 4 Hz.
Supplemental Figure S25. HMBC enhanced spectrum of SSDA in CD3OD with long range J filter width = 4 Hz.
Supplemental Figure S26. COSY spectrum of SSDA in CD3OD.
Supplemental Figure S27. COSY enhanced spectrum of SSDA in CD3OD with C6íH correlations.
Supplemental Figure S28. COSY enhanced spectrum of SSDA in CD3OD.
Supplemental Figure S29. TOCSY spectrum of SSDA in CD3OD.
Supplemental Figure S30. TOCSY enhanced spectrum of SSDA in CD3OD with C6íH correlations.
Supplemental Figure S31. TOCSY enhanced spectrum of SSDA in CD3OD.
Supplemental Figure S32. TOCSY enhanced spectrum of SSDA with view of C15-H correlations. Red circle represents missing correlation.
Supplemental Figure S33. HSQCíTOCSY enhanced spectrum of SSDA in CD3OD.
Supplemental Figure S34. HSQCíTOCSY enhanced spectrum of SSDA in CD3OD with C6íH correlations.
Supplemental Figure S35. HSQCíTOCSY enhanced spectrum of SSDA in CD3OD.
Supplemental Figure S36. HSQCíTOCSY enhanced spectrum of SSDA in CD3OD with spectral window.
Supplemental Figure S37. HSQCíTOCSY enhanced spectrum of SSDA in CD3OD with C21íH and C27íH correlations.
Supplemental Figure S38. Amidation of SSDA with EDC and ethanolamine and chromatogram of first amidation product of SSDA.
Supplemental Figure S39. Chromatogram of second amidation product of SSDA.
Supplemental Table S1. qNMR Results
Supplemental Table S2. qNMR Results and step-by-step Workflow 100% Method to Determine Purity
Supplemental Table S3. qNMR Results and step-by-step Workflow IC Method to Determine Purity
- Supplemental Data -