TY - JOUR
T1 - Enantiomeric separation and quantification of ephedrine-type alkaloids in herbal materials by comprehensive two-dimensional gas chromatography
AU - Wang, Min
AU - Marriott, Philip
AU - Chan, Wing-Hong
AU - Lee, Albert
AU - Huie, Carmen
PY - 2006
Y1 - 2006
N2 - The separation of ephedrine-type alkaloids and their enantiomers in raw herbs and commercial herbal products was investigated by carrying out enantioselective separation in the first-dimension column (containing P-cyclodextrin as the chiral selector) of a comprehensive two-dimensional gas chromatography (GC x GC) system, whereas a polar polyethylene glycol capillary column was used for separation in the second dimension. Naturally occurring ephedrine-type alkaloids and their synthetic analogues (enantiomeric counterparts) were adequately resolved from each other, as well as from potential interference species in the sample matrix using GC x GC, whereas single column GC analysis was unable to separate all the alkaloids of interest. Detection limits in the order of 0.1-1.3 mu g/mL and linearity of calibration with R-2 >= 0.999 over approximately the range of 0.5-100 mu g/mL for the quantitative determination of various ephedrine-type alkaloids were obtained. The commercial herbal products tested contained mostly (-)-ephedrine, (+)-pseudoephedrine, (-)-N-methylephedrine and (-)-norephedrine, with concentrations in the range of 40-2100, 0-1300, 15-300 and 0-30 mu g/g of the product, respectively, and repeatability of analysis was generally in the range of 1-5 . The present GC x GC method is effective and useful for the determination of the dosage levels of the principle ephedrine-type alkaloids in commercial health supplements and complex raw herb formulations, as well the differentiation of ephedrine-containing products that were derived from natural plant or synthetic sources, e.g., simply by visualizing the presence or absence of the enantiomeric pairs of () ephedrine and ()-N-methylephedrine in the GC x GC chromatograms.
AB - The separation of ephedrine-type alkaloids and their enantiomers in raw herbs and commercial herbal products was investigated by carrying out enantioselective separation in the first-dimension column (containing P-cyclodextrin as the chiral selector) of a comprehensive two-dimensional gas chromatography (GC x GC) system, whereas a polar polyethylene glycol capillary column was used for separation in the second dimension. Naturally occurring ephedrine-type alkaloids and their synthetic analogues (enantiomeric counterparts) were adequately resolved from each other, as well as from potential interference species in the sample matrix using GC x GC, whereas single column GC analysis was unable to separate all the alkaloids of interest. Detection limits in the order of 0.1-1.3 mu g/mL and linearity of calibration with R-2 >= 0.999 over approximately the range of 0.5-100 mu g/mL for the quantitative determination of various ephedrine-type alkaloids were obtained. The commercial herbal products tested contained mostly (-)-ephedrine, (+)-pseudoephedrine, (-)-N-methylephedrine and (-)-norephedrine, with concentrations in the range of 40-2100, 0-1300, 15-300 and 0-30 mu g/g of the product, respectively, and repeatability of analysis was generally in the range of 1-5 . The present GC x GC method is effective and useful for the determination of the dosage levels of the principle ephedrine-type alkaloids in commercial health supplements and complex raw herb formulations, as well the differentiation of ephedrine-containing products that were derived from natural plant or synthetic sources, e.g., simply by visualizing the presence or absence of the enantiomeric pairs of () ephedrine and ()-N-methylephedrine in the GC x GC chromatograms.
UR - http://www.sciencedirect.com/science/article/pii/S0021967305024222
U2 - 10.1016/j.chroma.2005.12.043
DO - 10.1016/j.chroma.2005.12.043
M3 - Article
SN - 0021-9673
VL - 1112
SP - 361
EP - 368
JO - Journal of Chromatography A
JF - Journal of Chromatography A
IS - 1-2
ER -