Má Huáng refers to Ephedra sinica Stapf and related species which contain norephedrine, norpseudoephedrine, ephedrine, pseudo-ephedrine, methylephedrine and methylpseudoephedrine. Ongoing safety evaluations of products which contain Má Huáng are hindered by lack of reliable analytical methods for these alkaloids. We have developed a solid phase extraction (SPE)/liquid chromatographic (LC) method for these alkaloids that can be utilized for both quantitation and confirmation. Products were extracted with diluted mobile phase and extracts prepared for analysis by SPE on a propylsulfonic acid (PRS) phase. Quantitative LC was performed on a 3.0 x 250 mm phenyl column using a mobile phase (MP) consisting of 93% buffer (150 mM ammonium acetate, 0.5% acetic acid)/7% CH3CN at a flow rate of 0.6 ml/min. LC/MS was performed on a Finnigan-MAT TSQ-7000 instrument with Atmospheric Pressure Chemical Ionization using a 2.0 x 250 mm phenyl column (MP as above) at a flow rate of 0.23 ml/min. The method provides baseline resolution of the 6 alkaloids and eliminates most of the interferences due to plant constituents which limit the usefulness of previously published methods.