女贞子HPLC指纹图谱及多指标成分测定

HPLC fingerprint and multi-component content determination of Ligustri lucidi Fructus

目的建立女贞子HPLC指纹图谱及多指标成分测定方法,为女贞子质量标准提升提供参考。方法采用HPLC法,以乙腈-0.1%甲酸水溶液梯度洗脱,体积流量1.0 m L/min,检测波长224 nm,建立女贞子指纹图谱,采用HPLC-Q/TOF-MS^E指认共有峰,并同时测定红景天苷、松果菊苷、特女贞苷、橄榄苦苷4种成分的量。结果建立了女贞子的HPLC指纹图谱,标定了14个共有峰,指认出其中12个色谱峰,10批样品相似度在0.994~1.000;红景天苷、松果菊苷、特女贞苷、橄榄苦苷4个被测组分均达到基线分离,在线性范围内具有良好的线性关系,r均大于0.990,平均回收率分别为97.40%、98.99%、97.03%和100.55%。结论该方法准确可靠,重复性好,可有效地控制和评价女贞子的质量。

Objective To establish the HPLC fingerpint method for simultaneous determination of four representative components（salidroside, echinacoside, specnuezhenide and oleuropein） of Ligustri Lucidi Fructus, so as to provide a reference for the quality control. Methods The method was performed on an Diamonsil C_（18） anlytical column（250 mm × 4.6 mm, 5 μm） at the column temperature of 30 ℃. The gradient mobile phase consisted of acetonitrile（A）-0.1% formic acid（B） with a flow rate of 1.0 mL/min. The detection wavelengths were 224 nm. HPLC-Q/TOF-MS were used for identifing the common peaks. Results By studying comparatively the fingerprints of 11 samples, 14 common peaks have been confirmed. There were 12 common peaks were identified by HPLC-Q/TOF-MS^E. The similarity of 10 batches are greater than 0.990. Salidroside, echinacoside, specnuezhenide and oleuropein were baseline separated with good linearity relationships（r 〉0.999） between concentration and peak areas over the linear ranges. The average recoveries of the investigated compounds were 97.40%, 98.99%, 97.03%, and 100.55%, respectively. Conclusion The method is accurate, reliable and with good reproducibility. It could be used for quality control and evaluation of Ligustri Lucidi Fructus.