UPLC-ECD法同时测定不同产地女贞子中9种成分的含量

Simultaneous Determination of Nine Components in Ligustri Lucidi Fructus from Different Habitats by UPLC-ECD

建立超高效液相色谱-电化学检测法(UPLC-ECD)同时测定不同产地女贞子中羟基酪醇、原儿茶酸、酪醇、红景天苷、毛蕊花糖苷、特女贞苷、木犀草苷、橄榄苦苷、芦丁的方法。取女贞子药材粉末0.25 g经10 mL80%甲醇超声提取20 min,提取液再经0.22μm滤膜过滤后上样进行色谱分离。采用Waters ACQUITY UPLC BEH shield RP 18(2.1 mm×100 mm,1.7μm)色谱柱分离,以甲醇-50 mmol/L柠檬酸盐缓冲液为流动相,梯度洗脱,流速为0.4 mL·min^(-1),柱温为45℃,进样体积为1μL,电化学检测器检测,库伦检测池第一通道电压为450 mV,第二通道为700 mV。结果表明,9种化合物在各自的质量浓度范围内线性关系良好(R^(2)≥0.9993);仪器精密度、方法重复性、稳定性试验的RSD≤2.5%;平均加样回收率在97.9%~102.2%范围内,RSD在2.4%~4.6%范围内。研究所建立的方法快速、简便,灵敏度高,结果稳定可靠,可用于同时测定女贞子中9种化合物的含量,为女贞子的质量控制提供参考。

A method was devoloped for the determination of hydroxytyrosol,protocatechuic acid,tyrosol,salidroside,verbascoside,specnuezhenide,luteolin,oleuropein and rutin in Ligustri Lucidi Fructus from different habitats by ultra-high performance liquid chromatography-electrochemical detection(UPLC-ECD).Ligustri Lucidi Fructus powder(0.25 g)was extracted ultrasonically for 20 min with 10 mL of 80% methanol.The extract was filtered through microporous membrane of 0.22μm and then separeted by a Waters ACQUITY UPLC BEH shield RP 18(2.1 mm×100 mm,1.7μm)chromatographic column.Methanol-50 mmol·L^(-1) potassium citrate solution with gradient elution was employed as the mobile phase.The flow rate was 0.4 mL·min^(-1),the column temperature was maintained at 45℃ and the injection volume was 1μL.The potential of electrochemical detector was set at 450 mV in the first channel and 700 mV in the second channel.The results showed that the linearity of nine constituents was good in the range of their mass concentration(R^(2)≥0.9993).RSD of precision,repeatability,and stability(12 h)were less than or equal to 2.5%.The average recovery rates were from 97.9% to 102.2% and the RSD was in the range of 2.4%~4.6%.The method in this study was rapid,simple,sensitive,stable and reliable.It could be applied for simultaneous determination of nine components in Ligustri Lucidi Fructus,which would provide a reference for the quality control of Ligustri Lucidi Fructus.