葛根枳椇软胶囊中黄酮类化合物的UPLC/Q-TOF-MS快速分析

Rapid analysis on flavonoids in Gegen Zhiju Soft Capsule by UPLC/Q-TOF-MS

目的采用UPLC/Q-TOF-MS技术对葛根枳椇软胶囊中的黄酮类成分进行定性分析。方法采用Agilent Poroshell120 SB-C18色谱柱（100 mm×2.1 mm,2.7μm）,以乙腈-0.1%甲酸溶液为流动相梯度洗脱,体积流量0.4 m L/min;质谱定性采用飞行时间质谱,电喷雾离子源,负离子模式下采集数据;质谱的相关参数：干燥气温度300℃,干燥气体积流量10 L/min,雾化气压力276 k Pa,鞘流气温度350℃,鞘流气流量11 L/min,毛细管电压3 500 V,碎片电压175 V。结果结合质谱数据及文献数据分析,鉴定出20个黄酮类化合物,相对分子质量集中于250~650。结论借助UPLC的快速分离和Q-TOF-MS测定的精确相对分子质量,可以有效地对葛根枳椇软胶囊中黄酮类成分进行分析鉴定。该方法准确、快速、灵敏,为其质量控制提供了实用可靠的技术手段。

Objective To identify the flavonoids in Gegen Zhiju Soft Capsule（a soft capsule prepared with Puerariae Radix and Hoveniae Dulcis Fructus seu Semen and so on） using ultra performance liquid chromatography coupled with quadrupole-time-offlight mass spectrometry（UPLC/Q-TOF-MS）. Methods The analysis was performed on Agilent Poroshell 120 SB-C18 column（100 mm × 2.1 mm, 2.7 μm） gradient elution with a mobile phase of 0.1% formic acid aqueous solution and acetonitrile. The flow rate was at 0.4 m L/min. TOFMS was applied for qualitative analysis, and the data were collected by the negative ion mode using ESI ion source. The parameters of ion source were as follows： drying gas temperature, 300 ℃; drying gas flow rate, 10 L/min; nebulizer gas pressure, 276 k Pa, sheath gas temperature, 350 ℃; sheath gas flow rate, 11 L/min; capillary voltage, 3 500 V; fragmentor voltage, 175 V. Results Twenty flavonoid compounds were identified by TOF-MS and literature data. Relative molecular weight was concentrated within 250—650. Conclusion The rapid separation with UPLC and Q-TOF-MS determination of the precise molecular weight information could effectively analyze and identify the flavonoid compounds in Gegen Zhiju Soft Capsule. The method is accurate, rapid, and sensitive, and could provide a reliable and effective technique for the quality control.