单标多组分HPLC定量分析法在川芎质量评价中的应用
Establishment and application of HPLC-QAMS for quality evaluation of Chuanxiong Rhizoma
-
摘要: 采用高效液相色谱法, 以丁烯基苯酞为内参物, 建立川芎中1种酚酸类成分和5种苯酞类成分的单标多组分HPLC定量分析方法, 并考察和验证该方法在川芎质量评价中应用的可行性和准确性.实验所用流动相为乙腈-0.2% 甲酸水溶液, 流速为1.0 mL·min-1, 柱温30 ℃, 检测波长分别为252 nm (阿魏酸、藁本内酯、丁烯基苯酞) 和266 nm (洋川芎内酯I、洋川芎内酯A、阿魏酸松柏酯), 进样量20 µL, 梯度洗脱.结果显示, 单标多组分HPLC定量分析法计算所得值与外标法实测值之间无显著性差异, RSD值均小于5%; 相对校正因子的耐用性较好, 色谱条件改变后, 相对校正因子变化的RSD值均小于5%.所建立的单标多组分HPLC定量分析法可准确地用于中药川芎的多指标同步质量控制.Abstract: A quantitative analysis method of multi-components with a single marker (QAMS) for simultaneous determination of six marker compounds (one from phenolic acids and five from phthalides) in Chuanxiong Rhizoma was established by applying HPLC and using butylidenephthalide as the internal reference substance. And also the feasibility and accuracy of the established method for quality evaluation and application of Chuanxiong Rhizoma were investigated and validated. The analysis was performed with the mobile phase consisting of acetonitrile - 0.2% aqueous formic acid. The flow rate was 1.0 mL·min-1 and the column temperature was maintained at 30 ℃. The detection wavelengths were set at 252 nm (for ferulic acid, Z-ligustilide, and butylidenephthalide) and 266 nm (for senkyunolide I, senkyunolide A, and coniferyl ferulate), separately, and 20 µL was injected for analysis with gradient elution. The results showed that there were no significant differences observed between the HPLC-QAMS method and the external standard method (RSD < 5%). The relative correction factors were credible (RSD < 5%) in changed chromatographic conditions. The established HPLC-QAMS method can be accurately used for simultaneously evaluating and controlling the quality of Chuanxiong Rhizoma with multi-components.
下载: