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KMID : 0903520050480030267
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Journal of the Korean Society of Agricultural Chemistry and Biotechnology
2005 Volume.48 No. 3 p.267 ~ p.272
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Quantitative Analysis of t-Cinnamaldehyde of Cinnamomum cassia by 1H-NMR Spectrometry
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Song Myoung-Chong
Yoo Jong-Su
Baek Nam-In
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Abstract
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trans-Cinnamaldehyde, a major component of Cinnamomum cassia, was quantitatively analyzed using the 1H-NMR spectrometry. Applicability of this method was confirmed through observing the variation of chemical shift in the 1H-NMR spectrum of t-cinnamaldehyde and the integration value according to various sample concentrations or running temperatures. When the 1H-NMR spectrometry was run for t-cinnamaldehyde (7.1429 mg/ml) at 19, 25, 30, 40 and 50oC, the chemical shifts of the doublet methine signal due to an aldehyde group were observed at 9.7202, 9.7184, 9.7169, 9.7142 and 9.7124 ppm, respectively, to imply that the running temperature had no significant variation in the chemical shift of the signal. The integration values of the signal were 1.37 (19oC), 1.37 (25oC), 1.37 (30oC), 1.37 (40oC) and 1.37 (50oC), respectively, to also indicate running temperature gave no effect on the integration value. When the sample solutions with various concentrations such as 0.4464, 0.8929, 1.7857, 3.5714, 7.1429 and 14.286 mg/ml were respectively measured for the 1H-NMR at 25oC, the chemical shifts of the aldehyde group were observed at 9.7206, 9.7201, 9.7196, 9.7192, 9.7185 and 9.7174 ppm. Even though the signal was slightly shifted to the high field in proportion to the increase of sample concentration, the alteration was not significant enough to applicate this method. The calibration curve for integration values of the doublet methine signal due to the aldehyde group vs the sample concentration was linear and showed very high regression rate (r2= 1.0000). Meantime, the 1H-NMR spectra (7.1429 mg/ml CDCl3, 25oC) of t-cinnamaldehyde and t-2-methoxycinnamaldehyde, another constituent of Cinnamomum cassia, showed the chemical shifts of the aldehyde group as δ H 9.7174 (9.7078, 9.7270) for the former compound and δ H 9.6936 (9.6839, 9.7032) for the latter one. The difference of the chemical shift between two compounds was big enough to be distinguished using the NMR spectrometer with 0.45 Hz of resolution. The contents of cinnamaldehyde in Cinnamomum cassia, which were respectively extracted with n-hexane, CHCl3, and EtOAc, were determiend as 94.2 mg/g (0.94%), 137.6 mg/g (1.38%) and 140.1 mg/g(1.40 %) t-cinnamaldehyde in each extract, respectively, by using the above method.
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KEYWORD
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1H-NMR, quantitative analysis, Cinnamomum cassia, t-cinnamaldehyde, t-2-methoxycinnamaldehyde
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