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高效液相色谱-质谱联用结合柱色谱法对藏药铁棒锤生物碱的研究

Study on the Alkaloids in Tibetan Medicine Aconitum pendulum Busch by HPLC-MSn Combined with Column Chromatography.

作者信息

Wang Beibei, Dong Jie, Ji Jiaojiao, Yuan Jiang, Wang Jiali, Wu Jiarui, Tan Peng, Liu Yonggang

机构信息

Beijing University of Chinese Medicine, Beijing 100102, China.

Beijing University of Chinese Medicine, Beijing 100102, China

出版信息

J Chromatogr Sci. 2016 May-Jun;54(5):752-8. doi: 10.1093/chromsci/bmw002. Epub 2016 Feb 18.

Abstract

A rapid, convenient and effective identification method of alkaloids was established and an attempt on isolating and analyzing the alkaloids in Aconitum pendulum Busch was conducted successfully. In this article, four high-content components including deoxyaconitine, benzoylaconine, aconine and neoline were isolated by using column chromatography. HPLC-MS(n)was employed to deduce the regulations of fragmentation of diterpenoid alkaloids which displayed a characteristic behavior of loss of CO(28u), CH3COOH(60u), CH3OH(32u), H2O(18u) and C6H5COOH(122u). Then, according to fragmentation regulation of mass spectrometry, 42 alkaloids were found inA. pendulum Among them, 38 compounds were identified and 29 alkaloids were reported for the first time for this herb. Therefore, this means that HPLC-MS(n)combined with column chromatography could work as an effective and reliable tool for rapid identification of the chemical components of herbal medicine.

摘要

建立了一种快速、便捷、有效的生物碱鉴定方法,并成功尝试对铁棒锤中的生物碱进行分离和分析。本文通过柱色谱法分离出了脱氧乌头碱、苯甲酰乌头原碱、乌头碱和尼奥灵四种高含量成分。采用高效液相色谱-质谱联用技术(HPLC-MS(n))推导二萜生物碱的裂解规律,其呈现出失去CO(28u)、CH₃COOH(60u)、CH₃OH(32u)、H₂O(18u)和C₆H₅COOH(122u)的特征行为。然后,根据质谱裂解规律,在铁棒锤中发现了42种生物碱。其中,鉴定出38种化合物,29种生物碱为本草首次报道。因此,这意味着HPLC-MS(n)结合柱色谱法可作为快速鉴定草药化学成分的有效且可靠的工具。

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