Wei Xiaodong, Shen Hongling, Wang Lijun, Meng Qingyan, Liu Wenjie
College of Life Science, Tarim University, Alar, Xinjiang 843300, China.
Key Laboratory of Protection and Utilization of Biological Resources in Tarim Basin of Xinjiang Production and Construction Corps, Alar, Xinjiang 843300, China.
J Anal Methods Chem. 2016;2016:9752735. doi: 10.1155/2016/9752735. Epub 2016 Sep 19.
A comprehensive two-dimensional (2D) reverse phase (RP) liquid chromatography (LC) method is developed for alkaloid analysis. This offline comprehensive 2D method is developed using different pH values. With a pH value of 10.5, most alkaloids appear in the form of neutral molecules possessing high retention factors based on their polarity, while the alkaloid polarity order is changed when the pH value decreased to 3.0. The performance of pH modulated 2D LC is demonstrated with 8 alkaloid standards which resulted in orthogonal separation. The developed method is then applied to total alkaloid separation in . The first-dimension separation is carried out using methanol and water containing 1.0% ammonium hydroxide and a strong base-resistant RP column, which afforded a peak capacity of 94. The second-dimension analysis is carried out with a surface positive charge column providing a peak capacity of 205 using a mobile phase consisting of acetonitrile and water with 0.15% formic acid. 2D analyses of total alkaloid extract from afford a total peak capacity of 9090. Sixteen compounds were tentatively identified based on their ultraviolet spectrum and MS/MS analyses. The proposed method provides an alternative approach to achieve high peak capacity for analysis of alkaloid extract.
开发了一种用于生物碱分析的综合二维（2D）反相（RP）液相色谱（LC）方法。这种离线综合二维方法是在不同pH值下开发的。在pH值为10.5时，大多数生物碱以中性分子的形式出现，基于其极性具有高保留因子，而当pH值降至3.0时，生物碱的极性顺序会发生变化。用8种生物碱标准品证明了pH调制二维液相色谱的性能，实现了正交分离。然后将所开发的方法应用于[具体植物名称]中总生物碱的分离。一维分离使用含有1.0%氢氧化铵的甲醇和水以及耐强碱的反相柱进行，其峰容量为94。二维分析使用表面带正电荷的柱进行，使用由乙腈和含有0.15%甲酸的水组成的流动相，峰容量为205。[具体植物名称]总生物碱提取物的二维分析提供了9090的总峰容量。基于紫外光谱和MS/MS分析初步鉴定了16种化合物。所提出的方法为实现生物碱提取物分析的高峰容量提供了一种替代方法。
