一测多评法同时测定杞菊地黄口服液中4种有效成分的含量

目的：建立以马钱苷为内参物，同时测定杞菊地黄口服液中莫诺苷、马钱苷、山茱萸新苷和丹皮酚含量的一测多评法（QAMS法）。方法：采用高效液相色谱法，使用C₁₈（250 mm×4.6 mm，5 μm）色谱柱，以乙腈（A）-0.3%磷酸水溶液（B）为流动相，梯度洗脱，柱温35℃，检测波长240 nm（0~79 min，检测莫诺苷、马钱苷和山茱萸新苷）、274 nm（80~95 min，检测丹皮酚）。以马钱苷为内参物，建立其与莫诺苷、山茱萸新苷和丹皮酚的相对校正因子（RCF），并进行含量计算，实现一测多评；同时采用外标法（ESM）测定杞菊地黄口服液中4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、丹皮酚的相对校正因子分别为1.048、1.390、0.349。建立的相对校正因子重现性良好，采用一测多评法测定的4批杞菊地黄口服液中各成分的含量范围分别为莫诺苷0.425~0.529 mg·mL^-1，马钱苷0.209~0.235 mg·mL^-1，山茱萸新苷0.045~0.072 mg·mL^-1，丹皮酚0.468~0.573 mg·mL^-1；各批样品中4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杞菊地黄口服液的质量是可行的。

Objective: To establish a QAMS method for simultaneous multi-components determination of four active components in Qijudihuang oral liquid with loganin as the internal reference, and to validate its feasibilities.Methods: The separation was carried out on a C₁₈ column(250 mm×4.6 mm, 5 μm)with the mobile phase consisting of acetonirtile(A)-0.3% phosphoric acid solution(B)at a flow rate of 1.0 mL·min^-1. The column temperature was 35℃. The detection wavelengths were changeable(0-79 min, 240 nm for detection of morroniside, loganin and cornuside; 80-95 min, 274 nm for detection of paeonol). The QAMS for Qijudihuang oral liquid was established and validated and loganin was selected as the internal reference substance. The relative correction factors(RCFs)of morroniside, cornuside and paeonol were calculated. The contents of four 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, cornuside and paeonol with reference to loganin were 1.048, 1.390, and 0.349, respectively, and the repeatability was good in different experimental conditions; The contents of four components in four batches of Qijudihuang oral liquid were determined by QAMS. The results are as follows:morroniside 0.425-0.529 mg·mL^-1, loganin 0.209-0.235 mg·mL^-1, cornuside 0.045-0.072 mg·mL^-1 and paeonol 0.468-0.573 mg·mL^-1, respectively. The quantitative results of both external standard method and QAMS for the four components in 4 batches of QijuDihuangOral Liquid were basically identical.Conclusion: The QAMS method established in this study is accurate and feasible to control the quality of Qijudihuang oral liquid.

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