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.
Marchei
Emilia
E
Drug Control and Evaluation Department, Istituto Superiore di Sanitá, V.le Regina Elena 299, 00161 Rome, Italy.
Pellegrini
Manuela
M
Pacifici
Roberta
R
Zuccaro
Piergiorgio
P
Pichini
Simona
S
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