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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.

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. suitable for GC

Materials

analytical column

Product No.
Description
Pricing

Astec® CHIRALDEX G-DM Capillary GC Column

L × I.D. 30 m × 0.25 mm, df 0.12 μm

mobile phase component

Product No.
Description
Pricing

Pentafluoropropionic anhydride

for GC derivatization, LiChropur, 99%

standard

Product No.
Description
Pricing

1,3-Dimethylamylamine

analytical 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