Gas Chromatographic Method for Analysis of p-Synephrine in Citrus aurantium L. Products

A method has been developed and validated for the identification and quantification of p-synephrine in Citrus aurantium L. products. The approach comprises GC-FID analysis followed by GC-MS confirmation after clean-up by solid phase extraction with a strong cation-exchange phase and derivatization w...

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Bibliographic Details
Published in:Chromatographia 2009-06, Vol.69 (2), p.225-229
Main Authors: Andrade, Adriana S, Schmitt, Gabriela C, Rossato, Luciana G, Russowsky, Dennis, Limberger, Renata P
Format: Article
Language:English
Subjects:
Analytical Chemistry
Chemistry
Chemistry and Materials Science
Chromatography
Full Short Communication
Laboratory Medicine
Pharmacy
Proteomics
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Summary:A method has been developed and validated for the identification and quantification of p-synephrine in Citrus aurantium L. products. The approach comprises GC-FID analysis followed by GC-MS confirmation after clean-up by solid phase extraction with a strong cation-exchange phase and derivatization with cyclohexanone. Oxazolidine derivative of p-synephrine was subjected to analysis by nuclear magnetic resonance (¹H and ¹³C NMR), GC-FID and GC-MS. The GC method was validated and was found to be linear in the range of 125-500 mg%. Intra-day and inter-day precisions were 3.60 and 3.59%, respectively. Mean recovery from extract of C. aurantium was 78.1 ± 3.64%. The selectivity of the method was further improved by confirmation of oxazolidine derivative of p-synephrine by GC-MS.
ISSN:0009-5893
1612-1112
DOI:10.1365/s10337-009-0991-5