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Gas Chromatographic Method for Analysis of p-Synephrine in Citrus aurantium L. Products
Authors:Andrade  Adriana S  Schmitt  Gabriela C  Rossato  Luciana G  Russowsky  Dennis  Limberger  Renata P
Institution:1.Programa de Pós-Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Av. Ipiranga, 2752, Porto Alegre, RS, Cep: 90610-000, Brazil
;2.Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves, 9500, Porto Alegre, RS, Cep: 91501-970, Brazil
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Abstract: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.
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