液相色谱-电喷雾电离-离子迁移谱联用法测定中药口服液中7种指标性成分

采用液相色谱-电喷雾电离-离子迁移谱联用技术,研究建立了中药口服液中丹参素、甘草酸、天麻素、绿原酸、葛根素、黄芩苷、芦丁等7种指标性成分的二维分离分析方法。样品溶液首先经ACQUITY UPLC BEH C18 色谱柱(50 mm×1 mm, 1.7 μm)分离后,导入可调节式分流器(分流比50∶1),柱后流出液分别进入离子迁移谱和三重四极杆质谱检测。分别详细优化了液相色谱、喷雾电压、迁移管和气体预加热温度、漂移气流速等实验条件,同时建立了指标性成分的液相色谱-三重四极杆质谱确证方法。7种中药指标性成分的检出限为2~10 μg/mL ,定量限为5~25 μg/mL 。采用本方法对中药口服液实际样品进行了检测分析。通过将液相色谱和离子迁移谱进行偶联,可实现目标化合物同时基于疏水性和离子迁移率差异的二维分离,获得更为丰富的测试信息。

Determination of seven indicative ingredients in oral liquids of Chinese medicine by liquid chromatography-electrospray ionization-ion mobility spectrometry

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 C₁₈ 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.