双标多测法Ⅲ-4种定性定量模式及紫外-可见光谱、质谱辅助定性

目的 ：以建立乳香中11-羰基-β-乙酰乳香酸(AKBA)和11-羰基-β-乳香酸(KBA)的含量测定法为例，探讨双标多测法的多种定性定量模式和色谱峰辅助定性方法。 方法：使用HPLC-PDA色谱仪建立含量测定法，以AKBA为参照物考察不同检测波长、流动相比例和pH下KBA的相对斜率(相对校正因子的倒数)变异情况，考察在10根不同C₁₈色谱柱上使用AKBA和乳香对照药材定性KBA的准确度。 结果：含量测定方法的线性和回收率均良好。以AKBA为参照物，KBA的相对斜率平均值为0.920，且在不同条件下保持稳定。使用AKBA和乳香对照药材结合紫外光谱定性KBA色谱峰的准确度高。 结论：建立的乳香双标多测法为乳香及含乳香制剂提供了一种有效且成本低廉的含量测定方法模式；4种不同的定性定量模式具有良好的实用性和可行性，扩展了双标多测法的适用范围。

Objective: To establish an HPLC method for determination of 11-keto-β-acetyl-boswellic acid(AKBA) and 11-keto-β-boswellic acid(KBA) in frankincense,and explore multiple qualitative and quantitative types of two reference substances for determination of multiple components(TRSDMC). Methods :The samples were separated by the HPLC-PDA instrument for determination of AKBA and KBA.The relative standard deviations of KBA's relative slope(reciprocal of relative correction factors) were calculated on different detection wavelengths,at mobile phase ratios and pH values using AKBA as the reference.The accuracies for identification chromatographic peak of KBA were calculated on 10 different C₁₈ columns with AKBA and the reference substance of crude drug. Results: The quantitative analysis was demonstrated with good linear relationship and recoveries.The average relative slope of KBA was 0.920 and showed good stability under different HPLC conditions.The qualitative analysis for KBA chromatographic peak was accurate using AKBA,the reference substance of crude drug in combination with UV spectrum. Conclusion: It is demonstrated that TRSDMC method established is accurate,economical,and suitable for determination of frankincense and its preparations.And the four qualitative and quantitative types of TRSDMC method are suitable and practical for quality evaluation of traditional Chinese medicine.