Application of gas chromatography-mass spectrometry for the detection of impurities in chlorogenic and caffeic acids

Hydroxycinnamic acids, including caffeic and chlorogenic acids, are widely found in plant extracts and demonstrate significant biological activity, making them promising for pharmaceutical and food industry applications. However, their natural origin and tendency to degrade during storage requires quality control, including the identification of impurities and degradation products. This study explores the potential of gas chromatography – mass spectrometry (GC-MS) for the analysis of pure caffeic and chlorogenic acid samples in order to detect impurities of various origins. It demonstrates that GC-MS analysis of acids without derivatization is not feasible due to the high polarity and thermal instability of the compounds under study, which leads to their decomposition under chromatography conditions. To improve volatility and thermal stability, derivatization was performed using N,O-bis(trimethylsilyl)trifluoroacetamide in the presence of trimethylchlorosilane, which increased the method’s sensitivity. Mass spectral analysis of the derivatized samples, supported by library searches, revealed the presence of various cinnamic acid derivatives, as well as an unidentified peak, presumably corresponding to the trimethylsilyl derivative of trihydroxycinnamic acid. The results demonstrate the effectiveness of GC-MS with prior derivatization for the detailed analysis of pure hydroxycinnamic acids and confirm its suitability for quality control and stability studies of these compounds.

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