Rapid selective screening and determination of ephedrine alkaloids using GC-MS footnote mark.
Ephedra (ma huang) has been widely used as an herb or herbal extract in both traditional Chinese medicine and Western world dietary supplements. The effects of Ephedra have been attributed to a series of six ephedrine alkaloids including ephedrine and pseudoephedrine. A GC-MS method for the ephedrine alkaloids is described which couples ammoniacal chloroform as the extraction solvent with a two-stage derivatisation scheme. This scheme produces the O-trimethylsilyl, N-trifluoracetyl derivatives (O-TMS, N-TFA) for the primary and secondary amine alkaloids, and the O-TMS derivatives for the tertiary amine alkaloids. Relatively clean extracts are obtained from complex matrices, and the six ephedrine alkaloids are effectively separated and identified. This approach was also evaluated for quantitative analysis, and was shown to provide quantitative results for ephedrine and pseudoephedrine, and good estimates for the four minor alkaloids. Figures of merit are presented for linearity, detection limits, precision and accuracy. We have applied this approach to the rapid screening and profiling of the ephedrine alkaloids in whole Ephedra plants, liquid plant extracts, dried powder plant extracts and a variety of Ephedra-containing dietary supplements.
Ranieri
Tracy L
TL
Forensic Chemistry Center, US Food and Drug Administration, 6751 Steger Dr., Cincinnati, OH 45231, USA.
Ciolino
Laura A
LA
D000470:Alkaloids / Q000032:analysis* / Q000737:chemistry; D019587:Dietary Supplements / Q000032:analysis; D029790:Ephedra sinica / Q000737:chemistry*; D004809:Ephedrine / Q000032:analysis* / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000032:analysis / Q000737:chemistry; D054199:Pseudoephedrine / Q000032:analysis / Q000737:chemistry; D012680:Sensitivity and Specificity
D000470:Alkaloids; D004364:Pharmaceutical Preparations; D054199:Pseudoephedrine; D004809:Ephedrine