GC Analysis of 1,3-Dimethylamylamine (DMAA) Enantiomers (N-Pentafluoropropionyl Derivatives) in a Sports Supplement on Astec® [TN="CHIRALDEX"] G-DM, 30 ºC Oven Temp.
Materials
analytical column
mobile phase component
standard
CONDITIONS
column
Astec CHIRALDEX G-DM, 30 m x 0.25 mm I.D., 0.12 μm particles (77033AST)
oven
30 °C (isothermal)
inj. temp.
250 °C
detector
FID, 250 °C
carrier gas
helium, 1 mL/min, constant
injection
1.0 μL 100:1 split
Description
Analysis Note
1,3-Dimethylamylamine (DMAA) is a stimulant found in various health supplements. Although often labelled as "natural," derived from geranium plants, it is suspected of actually having synthetic origins. If synthetic, then the supplement would fall under FDA regulations. In this study, chiral GC was used to measure the enantiomeric and diastereomeric ratios of synthetic DMAA. Shown here are the two sets of enantiomers of DMAA extracted from a sports supplment and separated by GC on Astec CHIRALDEX G-DM.
Other Notes
200 mg of supplement powder was dissolved in 1 mL water. 5 mg of internal standard was spiked into the solution. The pH was adjusted to 9–10 with sodium carbonate. 1 mL dichloromethane was added to the solution and vortexed. The whole solution was filtered with a syringe filter and the organic layer was collected and dried with magnesium sulfate. The dichloromethane solution was transferred to a 3 mL screw-top vial to which 0.5 mL PFPA was added and the vial sealed by cap with silicone rubber insert. The solution was heated for 30 min at 50 °C. Then the solvent and residual PFPA were removed at room temperature under reduced pressure. The sample was diluted with heptane and ready for GC injection.
Legal Information
Astec is a registered trademark of Merck KGaA, Darmstadt, Germany