丹参总酚酸提取物UPLC指纹图谱及成分定性研究

目的: 建立丹参总酚酸提取物的超高效液相色谱(UPLC)指纹图谱方法,并采用电喷雾离子源-四极杆-飞行时间质谱(ESI-Q-TOF MS)对其化学成分进行定性分析。 方法: 采用UPLC色谱系统,HSS T3色谱柱(2.1 mm×100 mm,1.7 μm);流动相为乙腈-0.1%甲酸水溶液,梯度洗脱;流速0.4 mL·min^-1;检测波长286 nm。质谱检测采用负离子V模式;电压2.5 kV;离子源温度100 ℃;雾化温度300 ℃;雾化气600 L·h^-1。 结果: 本方法在10 min内完成1次丹参总酚酸提取物的指纹图谱分析,各主要成分峰分离度良好,方法精密度、重复性的RSD均小于1.0%。对指纹图谱中的15个主要成分峰进行了鉴定,分别为丹参素、原儿茶醛、咖啡酸、丹酚酸F、丹酚酸H/L、丹酚酸G、丹酚酸D、丹酚酸E、迷迭香酸、紫草酸、丹酚酸B、异丹酚酸B/E、丹酚酸C和丹酚酸A。 结论: 本方法实现了丹参总酚酸提取物指纹图谱的快速、高效测定,同时解析了提取物中的化学组成,为高效、快速、全面控制其质量提供了基础。

Objective: To establish a UPLC method for fingerprint analysis of Salvia total phenolic acids,and qualitatively analyze its chemical constituents. Methods: The sample was conducted by UPLC with a Waters HSS T3 column (2.1 mm×100 mm,1.7 μm).The mobile phase consisted of acetonitrile and 0.1% formic acid with gradient elution at the flow rate of 0.4 mL·min^-1,and the detection wavelength was set at 286 nm.Negative-ion V mode was selected for qualitative analysis.The capillary voltage was set to 2.5 kV,the nebulization gas was set to 600 L·h^-1at a temperature of 300 ℃,and the source temperature was 100 ℃. Results: The main peaks were clearly separated in 10 min.The RSDs of precision and reproducibility were all less than 1.0%.Fifteen compounds were identified (tanshinol,protocatechualdehyde,caffeic acid,rosmarinic acid,lithospermic acid,salvianolic acid F,H/L,G,D,E,B,A,and isosalvianolic acid F,B/E). Conclusion: The high-performance and rapid method is successfully used to fingerprint analysis,and the chemical constituents are also identified.

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