Fang Kang, Guo Xiangyu, Wang Hongwei, Xiong Xingchuang, Bai Hua, Lei Haimin, Ma Qiang
Chinese Academy of Inspection and Quarantine, Beijing 100176, China.
School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 102488, China.
Se Pu. 2019 Jul 8;37(7):742-749. doi: 10.3724/SP.J.1123.2019.01013.
A two-dimensional separation and analysis method, based on liquid chromatography-electrospray ionization-ion mobility spectrometry (LC-ESI-IMS), is developed for the determination of seven indicative ingredients (danshensu, glycyrrhizic acid, gastrodin, chlorogenic acid, puerarin, baicalin, and rutin) in oral liquids of Chinese medicine. The sample was first separated on an ACQUITY UPLC BEH C column (50 mm×1 mm, 1.7 μm). The post-column effluent was directed to an adjustable flow splitter with a split ratio of 50:1. The low-flow and high-flow outlets were connected to an ion mobility spectrometer and a triple quadrupole mass spectrometer, respectively. The experimental conditions for LC, spray voltage, drift tube temperature, gas pre-heating temperature, and drift gas velocity were systematically optimized. The limits of detection (LODs) and quantitation (LOQs) for the seven analytes were 2-10 μg/mL and 5-25 μg/mL, respectively. The proposed method was applied for the analysis of real oral liquids of Chinese medicine samples. By coupling LC and IMS, two-dimensional separation could be achieved based on hydrophobicity difference and ionic mobility disparity, thus providing more comprehensive measurement information than LC or IMS used alone.
建立了一种基于液相色谱 - 电喷雾电离 - 离子淌度谱（LC - ESI - IMS）的二维分离分析方法，用于测定中药口服液中的七种指示性成分（丹参素、甘草酸、天麻素、绿原酸、葛根素、黄芩苷和芦丁）。样品首先在ACQUITY UPLC BEH C柱（50 mm×1 mm，1.7 μm）上进行分离。柱后流出物导入分流比为50:1的可调分流器。低流量和高流量出口分别连接到离子淌度谱仪和三重四极杆质谱仪。对液相色谱、喷雾电压、漂移管温度、气体预热温度和漂移气体流速的实验条件进行了系统优化。七种分析物的检测限（LOD）和定量限（LOQ）分别为2 - 10 μg/mL和5 - 25 μg/mL。该方法应用于实际中药口服液样品的分析。通过联用液相色谱和离子淌度谱，基于疏水性差异和离子淌度差异可实现二维分离，从而比单独使用液相色谱或离子淌度谱提供更全面的测量信息。
