远志UPLC多指标成分的测定及指纹图谱研究

目的 建立远志超高效液相色谱(UPLC)多成分测定方法及指纹图谱方法。方法 采用UPLC法,以乙腈-0.1%甲酸水溶液梯度洗脱,体积流量0.4 m L/min,检测波长320 nm,测定24批远志药材中sibiricose A5、sibiricose A6、sibiricaxanthone B、glomeratose A、polygalaxanthone III、3,6′-disinapoyl sucrose 6种成分的量,并建立远志药材指纹图谱,采用超高效液相色谱-飞行时间质谱(UPLC-Q-TOF-MS~E)指认共有峰。结果 不同产地远志中3,6′-disinapoyl sucrose与sibiricose A6量差异较大;建立的药材UPLC指纹图谱共标定37个共有峰,指认出其中33个峰,24批样品相似度在0.756~0.997。成分量及相似度综合分析结果表明不同地区远志药材质量存在一定差异。结论 建立的测定结合指纹图谱分析方法可有效、全面地用于远志药材的质量评价。

Simultaneous analysis on index compounds and fingerprint analysis on Polygalae Radix by ultra performance liquid chromatography

Objective A rapid and specific ultra performance liquid chromatography (UPLC) method was established for simultaneous analysis on six compounds and fingerprint analysis on Polygalae Radix to evaluate the herb quality from different habitats in China. Methods The UPLC method was carried out by gradient elution with acetonitrile-formic acid water (0.1%). The flow rate was 0.4 mL/min. The detection wavelength was at 320 nm. The fingerprint chromatograms and the contents of six compounds including sibiricose A₅, sibiricose A₆, sibiricaxanthone B, glomeratose A, polygalaxanthone III, and 3,6''-disinapoyl sucrose in 24 batches of Polygalae Radix were analyzed. The common peaks were identified by ultra performance liquid chromatography tandem with time-of-flight mass spectrometry with MS^E data-acquistion mode (UPLC-Q-TOF-MS^E). Results There was a difference in contents of six compounds, especially for the content of 3,6''-disinapoyl sucrose and sibiricose A₆. Thirty-seven peaks were selected as the common peaks, of which 33 peaks were identified, and the similarities of 24 batches were between 0.756 and 0.997. Based on the results of quantification and fingerprint analysis, a certain difference between samples from different habitats was further proven. Conclusion The validated UPLC quantitative analysis and fingerprint methods are successfully used in the quality control of Polygalae Radix.