Digitalis purpurea Species Overview
Experiment: MPGR
Platform: Digitalis LC/TOF MS Positive Ion
| Instrument | |
| Manufacturer | Waters |
| Model # | LCT Premier |
| Operational software name & version | MassLynx v 4.1 |
| Ionization source | |
| Gas flows | Cone: 40 L/hr; Desolvation: 350 L/hr |
| Ionization mode | Electrospray |
| Polarity | Positive |
| Skimmer/focusing lens voltages | Aperture 1 voltage: 20 (Function 1); 40 (Function 2); 60 (Function 3); 80 (Function 4) |
| Vacuum pressure | ~2 mbar |
| Mass Analyzer | |
| Calibration, resolution | 8000 |
| Logic program for data acquisition | MassLynx |
| m/z range | 100-1400 |
| Mass accuracy | RMS residual 1.94e-3 amu; Mean residual: 1.20 e-3 amu |
| Spectral acquisition rate | Scan time: 0.15 sec |
| Type | orthogonal TOF |
| Vacuum pressure | ~7.88 e-7 mbar |
| Quality Control | |
| Mass accuracy | Calibrate before analysis of set of samples |
| Resolution | Tune every month |
| Sensitivity | Tune every month |
| Tune | Tune every month |
+ Chromatography Metadata
| Chromatography Instrument | |
| Liquid or Gas chromatography? | Liquid |
| Manufacturer | Shimadzu |
| Model number | Prominence High Performace Liquid Chromatograph (Degasser: DGU-20A5; Solvent Delivery: LC-20AD; Column Oven: CTO-20A |
| Software package | MassLynx |
| Version number or Date | 4.1 |
| Auto-injector | |
| injection volume | 10 microL |
| Injector model/type | Shimadzu (SIL-5000) |
| method name | NIH_Dig_37min_AscExp_001 |
| software version | MassLynx 4.1 |
| Separation column and pre/guard column | |
| Internal diameter of column | 0.21 cm |
| Length of column | 5 cm |
| Manufacturer | Supelco |
| Physical parameters | 2.7 microm |
| Product Name and catalogue number (year of ca | Ascentismicro Express C18 Analytical HPLC column; Catalogue number: 53822-U |
| Stationary media composition | C18 |
| Separation parameters | |
| For GC, thermal gradient profiles | N/A |
| For LC, solvent gradient profile | an elution gradient starting at 95% solvent A and 5% solvent B for 1 min, then to 25% solvent A in 20 min, 5% solvent A in 5 min, 0% solvent A in 30 min, 50% solvent A in 31 and 95% solvent A in 37 min |
| GC injector temperature | N/A |
| Method name | NIH_Digitalis_37min_AscExp_001 |
| Mobile phase composition | 10 mM ammonium formate, pH 2.85 (A) and 1:2 v/v Acetonitrile/Isopropanol (B) |
| Mobile phase flow rate | 0.3 mL/min |
| Quality Control | |
| Do you estimate/determine chromatographic res | No |
| Do you use validation sample? If yes, what is | 12.5 microM mixture of the standards followed by blank for every 20 samples |
| Internal standards: What is its chemical nam | None, other than 4-hydroxypropyl benzoate added during extraction |
| Age of column (in chromatography cycles) | |
| Age of septum (in chromatography cycles) | N/A |
| Frequency of blank chromatograms | Beginning of each run and after the standards |
| Data acquisition | |
| Date | 4/8/10 |
| Date of analysis | 4/10/10 |
| Deviations from SOP | None |
| Operator | Shawn Shadkami |
| SOP Protocol name | NIH_Dig_37min_AscExp_001 |
| SOP Protocol name | NIH_medplant_Digitalis_esipos_W_37min_4funct |
Metabolite Search
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Chemically defined metabolites in this experiment:
Digitoxigenin bis-digitoxoside[M+NH4]+ FS-Dig-HPLC-E-POS-F1-652.422-4.8
Digitoxin; Digitoxoside
[M+NH4]+ FS-Dig-HPLC-E-POS-F1-782.477-10.51
Gitoxin; Gitoxoside
[M+NH4]+ FS-Dig-HPLC-E-POS-F1-798.469-9.37
Glucodigitoxin; Purpurea glycoside A
[M+NH4]+ FS-Dig-HPLC-E-POS-F1-944.536-9.33
Strospeside; Strospesid
[M+NH4]+ FS-Dig-HPLC-E-POS-F1-568.355-6.24