目的 通过高效液相色谱串联四极杆飞行时间质谱法（HPLC-Q-TOF-MS）鉴定广金钱草中主要活性成分，通过高效液相色谱-二极管阵列检测器（HPLC-DAD）法同时测定广金钱草中7种黄酮类成分（夏佛塔苷、异夏佛塔苷、维采宁-2、异荭草苷、异牡荆苷、木犀草素、芹菜素）的量。方法 采用Phenomenex Kinetex C₁₈色谱柱（4.6 mm×250 mm，5 μm），以甲醇（A）-0.2%甲酸水（B）为流动相梯度洗脱进行色谱分离，体积流量为1.0 mL/min，柱温40℃；Q-TOF-MS在电喷雾负离子模式下采集数据，分流比为1∶1；采用HPLC-DAD法定量，检测波长为272 nm。结果 采用HPLC-Q-TOF-MS法鉴定了广金钱草中的41种主要活性成分，其中包括37个黄酮类成分，4个酚酸类成分。成功建立了同时测定广金钱草中7种黄酮类成分的HPLC-DAD法，各成分的线性关系良好（r>0.999 0），精密度、重复性和稳定性良好，回收率在96.7%～102.4%（n=6），RSD均小于4.94%。结论 通过HPLC-Q-TOF-MS联用技术，为阐明广金钱草药效物质基础提供参考；建立的HPLC-DAD法同时测定广金钱草中7种黄酮类成分的定量分析方法简便、快捷、准确，为综合评价广金钱草的质量提供参考。

Objective This study is aimed to establish a high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometric (HPLC-Q-TOF-MS) method for analyzing the main active components in Desmodii Styraciflii Herba, and to establish an HPLC-DAD method for simultaneously determining its seven flavonoids compounds (schaftoside, isoschaftoside, vicenin-2, isoorientin, isovitexin, luteolin, and apigenin). Methods The analysis was performed on a Phenomenex Kinetex C₁₈ column with a gradient elution of methanol-0.2% aqueous formic acid at the flow rate of 1.0 mL/min. The column temperature was 40℃. The Q-TOF-MS discriminant analysis was performed under negative electrospray ion mode and the split ratio was 1:1. Quantitative analysis of seven compounds in Desmodii Styraciflii Herba was carried by HPLC-DAD. The determination wavelength was at 272 nm. Results Forty-one main active constituents were separated and identified by HPLC-Q-TOF-MS, including 37 flavonoids compounds and four phenolic acids. A HPLC-DAD method was successfully developed for determining seven flavonoids compounds. The standard curves for all seven compounds showed good linearity with correlation coefficients higher than 0.999 0 within the test ranges. The average recoveries (n=6) were between 96.7%-102.4%, and RSD≤4.94%. Conclusion Analyzing the main active components provides a significant guidance for the substance basis research of Desmodii Styraciflii Herba. The HPLC-DAD method for simultaneously determining seven flavonoids compounds is accurate, reproducible, and provides the basis for the quality control of Desmodii Styraciflii Herba.

国家中医药管理局项目（201507002）；广东省科技计划项目（产学研合作专项）（2015B090901033）