一测多评法测定左归丸中3种环烯醚萜苷类成分的含量

Quantitative Analysis of 3 Iridoid Glucosides in Zuigui Pills Using Single Marker by QAMS Method

目的:建立以马钱苷为内参物,同时测定左归丸中莫诺苷、马钱苷和山茱萸新苷含量的一测多评法(QAMS)。方法:采用高效液相色谱法,Phenomenex C18(250 mm×4.6 mm,5μm)硅胶色谱柱;流动相:乙腈(A)-0.3%磷酸水溶液(B)梯度洗脱;柱温35℃;检测波长(0~65 min,240 nm,检测莫诺苷和马钱苷;66~80 min,218 nm,检测山茱萸新苷)。以马钱苷为内参物,建立其与莫诺苷、山茱萸新苷的相对校正因子(RCFS),并进行含量计算,实现一测多评;同时采用外标法(ESM)测定左归丸中3种有效成分的含量,比较一测多评法计算值与外标法实测值的差异。结果:在一定线性范围内,马钱苷与莫诺苷、山茱萸新苷的相对校正因子分别为1.048、1.390。建立的相对校正因子重现性良好,7批左归丸中3种成分的计算值与实测值间无显著差异。结论:采用本研究建立的"一测多评"法控制左归丸的质量是可行的。

Objective： To establish a method for quantitative analysis of multi-components using single-marker（QAMS） for determination of 3 iridoid glucosides in Zuigui pills with loganin as the internal reference, and to validate its feasibility by the simultaneous quantitative assay of the 3 components. Methods： The separation was carried out on a Phenomenex C18 Silica gel column（250 mm×4.6 mm, 5 μm）, and the mobile phase consisted of acetonitrile（A）-0.3% phosphoric acid solution（B） at a flow rate of 1.0 m L·min-1, with the column temperature of 35℃. The detection wavelengths were changeable（0-65 min, 240 nm for detection of morroniside and loganin; 66-80 min, 218 nm for detection of cornuside）. The QAMS for Zuigui pills was established and validated and loganin was selected as the internal reference substance. The relative correction factors（RCFs） of morroniside and cornuside were calculated. The contents of 3 components were determined by both external standard method and QAMS. The validity of the QAMS method was evaluated by comparison of the quantitative results of both methods. Results： RCFs of morroniside and cornuside with reference to loganin were respectively 1.048 and 1.390, and the repeatability was good in different experimental conditions; the quantitative results of both external standard method and QAMS for the 3 components in 7 batches of Zuigui pills were basically identical. Conclusion： The QAMS method established in this research is accurate and feasible to control the quality of Zuigui pills.