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Forced Degradation of Cannabidiol CBD

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Forced Degradation of Cannabidiol CBD ( forced-degradation-cannabidiol-cbd )

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[ APPLICATION NOTE ] EXPERIMENTAL METHODS Conditions UPLC Reversed-Phase Method UPC2 Method (Figure 7, Figure 8, and Figure 9) Analytical column: Analytical flow rate: Mobile phase A: Mobile phase B: Gradient: Oven temp.: PDA detector: MS detector: Injection volume: Software: ACQUITY UPLC CSH C18, 130Å, 1.7 μm, 2.1 x 150 mm (p/n 186005298) 0.60 mL/min Water Acetonitrile Starting conditions at 73% mobile phase B with a 1 minute hold time, linear increase to 90% mobile phase B over 6 minutes 30 °C Wavelength 225 nm at 4.8 nm resolution, 3D data scan range Wavelength 225 nm at 4.8 nm resolution, scan range 200–400 nm ACQUITY QDa ionization mode ESI+ mass range 100–600 Da, cone voltage 15 V, capillary temperature 500 °C, capillary voltage 0.80 kV 2 μL Empower3 Chromatography Data Software Analytical column: Analytical flow rate: Mobile phase A: Mobile phase B: Gradient: ABPR: Oven temp.: PDA detector: MS detector: Make up solvent: Injection volume: Software: Trefoil Cel1, 2.5 μm, 3.0 x 150 mm (p/n 186007464) 2.0 mL/min CO2 200 proof ethanol Starting conditions at 3% mobile phase B, linear increase to 13% mobile phase B over 9 minutes 1800 psi 50 °C Wavelength 225 nm at 4.8 nm resolution, Compensated reference 310–410 nm, 3D data scan range 200–400 nm ACQUITY QDa ionization mode ESI+ mass range 100–600 Da, cone voltage 10 V, capillary temperature 550 °C, capillary voltage 1.5 kV 8:2 methanol/water with 0.1% formic acid at 0.75 mL/min 2 μL Empower3 Chromatography Data Software Solvents, Standards and Samples Approximately 165 mg of crystalline CBD were dissolved in exactly 10 mL of 190 proof ethanol. Three aliquots were prepared to contain 0.1 M acid, 0.1 M base, and 3.0% oxidizing agent. One aliquot was set aside to serve as the control. The samples were stored in glass vials and incubated at 60 °C for 24 hours. All solvents and diluents were HPLC-MS grade and filtered via 0.45-μm filters (p/n WAT200516). Reference standard solutions of cannabidiol (CBD) (p/n C6395), cannabinol (CBN) (p/n C6888), cannabichromene (CBC) (p/n C143), cannabigerol (CBG) (p/n C141), (±)Δ9-THC (p/n T-047), (-)Δ9-THC (p/n T-032) and (-)Δ8-THC (p/n T-032) were obtained from Sigma-Aldrich® Inc. Allentown, PA. Forced Degradation of Cannabidiol 2

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