An optimized and validated 1H NMR method for the quantification of α-pinene in essentials oils

Publication date: 1 April 2016
Source:Talanta, Volume 150
Author(s): Cristiane I. Cerceau, Luiz C.A. Barbosa, Claudinei A. Filomeno, Elson S. Alvarenga, Antônio J. Demuner, Paulo H. Fidencio
The authenticity and composition of commercial essential oils requires strict quality control. Due to the importance of α-pinene containing essential oils, a rapid and efficient method for quantification of this terpene in oils of eucalyptus, pink pepper and turpentine using ¹H NMR was developed and validated. All evaluated parameters (selectivity, linearity, accuracy/precision, repeatability, robustness, stability of analyte and internal standard in solutions) showed satisfactory results. The limit of detection (LOD) and limit of quantification (LOQ) were 0.1 and 2.5mg respectively. These values indicated that α-pinene was detected in 35mg samples containing at least 0.3% of this compound. In addition, a minimum of 8% of α-pinene in the sample was required for quantification. Furthermore, the standard deviations found in the ¹H NMR methodology were less than 1% and were lower than those obtained by gas chromatographic analysis. Statistical tests have shown that the results obtained by ¹H NMR methodology are similar to those obtained by GC-FID technique using external and internal standardization and normalization within 95% confidence. R&R values lower than 10% have shown that all the methods are appropriate and the ¹H NMR method is suitable for quantification of α-pinene in samples of essential oils since this method possessed the smallest R&R (1.81) value.

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