A rapid and simple procedure for the determination of ephedrine alkaloids in dietary supplements by gas chromatography-mass spectrometry.
A simple method for the determination of ephedrine alkaloids: ephedrine (EF), pseudoephedrine (PE), norpseudoephedrine (NPE), norephedrine (NE) and methylpseudoephedrine (MPE) in dietary supplements by gas chromatography-mass spectrometry is described. After the addition of 3,4-methylenedioxypropylamphetamine as internal standard, a liquid-liquid extraction procedure in alkaline conditions with chloroform/isopropanol (9:1, v/v) was applied to the samples prior to analysis. Chromatography was performed on a fused capillary column and analytes, derivatized with pentafluoropropionic anhydride, were determined in the selected-ion-monitoring (SIM) mode. The method was validated in the range 0.3-10 microg/mg for EP, 0.06-2.5 microg/mg for PE and NPE and 0.04-1 microg/mg NE and MPE. Mean recovery ranged between 65.7 and 81.3% for the different analytes in dietary supplements. The quantification limits were 0.3 microg/mg for EP, 0.06 microg/mg for PE, 0.04 microg/mg for NPE, NE and MPE. The method was applied to analysis of various dietary supplements containing Ma-huang (Ephedra Sinica) and Sida Cordifolia plant extracts promoted for aiding weight control and boosting sports performance and energy.
Drug Control and Evaluation Department, Istituto Superiore di Sanitá, V.le Regina Elena 299, 00161 Rome, Italy.
Emilia
E
Marchei
Manuela
M
Pellegrini
Roberta
R
Pacifici
Piergiorgio
P
Zuccaro
Simona
S
Pichini
D000470:Alkaloids / Q000032:analysis*; D002138:Calibration; D019587:Dietary Supplements / Q000032:analysis*; D029789:Ephedra / Q000737:chemistry*; D004809:Ephedrine / Q000032:analysis*; D005615:Freezing; D008401:Gas Chromatography-Mass Spectrometry; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results
D000470:Alkaloids; D004809:Ephedrine