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发展了一种高灵敏度的高效液相色谱-电化学检测(HPLC-ECD)方法,用于丹参中5种酚类物质的定量分析。为了获得较高的检测灵敏度,对流动相的pH、缓冲溶液类型和浓度、有机相种类和梯度以及流速做了系统研究。在较低的pH(2.8)、较低的缓冲盐浓度(20 mmol/L NaH2PO4)和较缓的乙腈梯度下,以0.2 mL/min流速可为5种酚类的分离检测提供较好的分离度和较高的检测灵敏度。在获得优化的分离参数后,将其用于14批丹参药材中5种酚类物质的定量分析。结果表明,该方法可获得较好的回收率(>95%)、较宽的线性范围(高达4个数量级)、较好的重复性(RSD<4.01%)和较高的灵敏度(咖啡酸的LOQ低至1.5μg/L)。与紫外检测方法相比,ECD检测方法具有更高的选择性,可减少非抗氧化活性的物质的干扰。
A high-sensitivity liquid chromatography-electrochemical detection (HPLC-ECD) method was developed for the quantitative analysis of five phenolic compounds in Salvia miltiorrhiza. In order to obtain higher detection sensitivity, the pH of the mobile phase, the type and concentration of buffer solution, the type and gradient of organic phase and the flow rate were studied systematically. At lower pH (2.8), lower buffer salt concentration (20 mmol / L NaH2PO4) and slower acetonitrile gradient, a 0.2 mL / min flow rate provides better separation of the five phenols Degree and high detection sensitivity. After obtaining the optimized separation parameters, it was used for quantitative analysis of five phenolic compounds in 14 batches of Salvia miltiorrhiza. The results show that the method achieves good recovery (> 95%), wide linear range (up to 4 orders of magnitude), better reproducibility (RSD <4.01%) and higher sensitivity (caffeic acid LOQ as low as 1.5 μg / L). Compared with the UV detection method, ECD detection method has a higher selectivity, can reduce the non-antioxidant activity of the material interference.