Hasada Keiko, Yoshida Takamitsu, Yamazaki Takeshi, Sugimoto Naoki, Nishimura Tetsuji, Nagatsu Akito, Mizukami Hajime
Graduate School of Pharmaceutical Sciences, Nagoya City University, 3-1 Tanabe-dori, Mizuho-ku, Nagoya, Japan.
J Nat Med. 2010 Apr;64(2):161-6. doi: 10.1007/s11418-010-0393-x. Epub 2010 Feb 19.
(1)H-NMR spectroscopy was successfully applied to the quantitative determination of atractylon in Atractylodis Rhizoma (dried rhizomes of Atractylodes ovata and A. japonica) and Atractylodis Lanceae Rhizoma (dried rhizomes of Atractylodes lancea and A. chinensis). The analysis was carried out by comparing the integral of the H-12 singlet signal of atractylon, which was well separated in the range of delta 6.95-7.05 ppm in the NMR spectrum, with the integral of a hexamethyldisilane (HMD) signal at delta 0 ppm. The atractylon contents obtained by the (1)H-NMR spectroscopy were consistent with those obtained by the conventional HPLC analysis. The present method requires neither reference compounds for calibration curves nor sample pre-purification. It also allows simultaneous determination of multiple constituents in a crude extract. Thus, it is applicable to chemical evaluation of crude drugs as a powerful alternative to various chromatographic methods.
(1)氢核磁共振波谱法已成功应用于白术(白术和日本白术的干燥根茎)和苍术(茅苍术和北苍术的干燥根茎)中苍术酮的定量测定。分析方法是将苍术酮的H-12单峰信号积分(该信号在核磁共振谱中δ 6.95 - 7.05 ppm范围内分离良好)与δ 0 ppm处六甲基二硅烷(HMD)信号的积分进行比较。通过氢核磁共振波谱法获得的苍术酮含量与通过传统高效液相色谱分析获得的结果一致。本方法既不需要用于校准曲线的参考化合物,也不需要样品预纯化。它还允许同时测定粗提取物中的多种成分。因此,作为各种色谱方法的有力替代方法,它适用于中药材的化学评价。