HPLC一测多评法测定乳宁颗粒中柴胡皂苷a、柴胡皂苷d、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_(A)、王不留行环肽A和王不留行环肽B  

Determination of saikosaponin a, saikosaponin d, 15, 16-dihydrotanshinone Ⅰ,cryptotanshinone, tanshinone Ⅰ, tanshinone Ⅱ_(A), segetalin A and segetalin B in Runing Granule by HPLC-QAMS

作　　者：李占芳 李俊卿 许伟 任强[2] 周金辉[2] LI Zhanfang;LI Junqing;XU Wei;REN Qiang;ZHOU Jinhui(Dongying Food and Drug Inspection Center,Dongying 257091,China;College of pharmacy,Jining Medical University,Rizhao 276800,China)

机构地区：[1]东营市食品药品检验中心,山东东营257091 [2]济宁医学院药学院,山东日照276800

出　　处：《药物评价研究》2021年第7期1434-1440,共7页Drug Evaluation Research

基　　金：山东省中医药科技发展计划项目(2019-0449)。

摘　　要：目的建立HPLC-一测多评(QAMS)法同时检测乳宁颗粒中柴胡皂苷a、柴胡皂苷d、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_(A)、王不留行环肽A、王不留行环肽B的含量。方法采用Agilent HC-C_(18)(250 mm×4.6 mm,5μm)色谱柱,柱温30℃;乙腈-0.1%磷酸为流动相,梯度洗脱,体积流量1.0 mL/min,检测波长分别为210 nm(检测柴胡皂苷a和柴胡皂苷d)和280 nm(检测二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_(A)、王不留行环肽A和王不留行环肽B)。以丹参酮ⅡA为内参物,建立其与柴胡皂苷a、柴胡皂苷d、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、王不留行环肽A、王不留行环肽B的相对校正因子(RCF),计算各成分含量,同时与外标法(ESM)实测值进行比较,以验证HPLC-QAMS法的可行性。结果柴胡皂苷a、柴胡皂苷d、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_(A)、王不留行环肽A、王不留行环肽B分别在4.08~102.00、2.97~74.25、0.74~18.50、1.56~39.00、1.98~49.50、3.69~92.25、0.66~16.50、0.54~13.50μg/mL(r≥0.9991)线性关系良好,平均加样回收率(RSD)分别为100.08%(0.54%)、99.68%(0.67%)、97.85%(1.64%)、98.99%(0.92%)、98.81%(1.35%)、100.06%(0.62%)、96.81%(0.73%)、97.79%(1.41%),乳宁颗粒中各成分一测多评法计算值与外标法实测含量值无显著性差异。结论所建立的HPLC-QAMS法为乳宁颗粒提供了一种准确可行的多指标质量控制模式。Objective To establish an HPLC-QAMS method for the determination of saikosaponin a, saikosaponin d, 15, 16-dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ, tanshinone Ⅱ_(A), segetalin A and segetalin B in Runing granule. Methods The samples were separated on an Agilent HC-C_(18)(250 mm × 4.6 mm, 5 μm), gradient elution conditions were the mobile phase using acetonitrile-0.1% phosphoric acid solution at a flow rate of 1.0 m L/min.The detection wavelength were 210 nm for saikosaponin a and saikosaponin d,and 280 nm for 15,16-dihydrotanshinone Ⅰ,cryptotanshinone,tanshinone Ⅰ,tanshinone Ⅱ_(A),segetalin A and segetalin B,the column temperature was 30 ℃.Using tanshinone Ⅱ_(A) as an internal standard,the relative correction factors of saikosaponin a,saikosaponin d, 15, 16-dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ, segetalin A and segetalin B were calculated, after which the content determination was made.The method was validated by comparison of the quantitative results between external standard method(ESM) and HPLC-QAMS method. Results Saikosaponin a, saikosaponin d, 15, 16-dihydrotanshinone Ⅰ, cryptotanshinone,tanshinone Ⅰ, tanshinone Ⅱ_(A), segetalin A and segetalin B showed good linear relationships within the ranges of 4.08 - 102.00,2.97 - 74.25, 0.74 - 18.50, 1.56 - 39.00, 1.98 - 49.50, 3.69 - 92.25, 0.66 - 16.50 and 0.54 - 13.50 μg/m L(r ≥ 0.999 1),whose average recoveries(RSD) were 100.08%(0.54%), 99.68%(0.67%), 97.85%(1.64%), 98.99%(0.92%), 98.81%(1.35%),100.06%(0.62%), 96.81%(0.73%), 97.79%(1.41%), respectively. No significant differences were found in the quantitative analysis of components by ESM and HPLC-QAMS method. Conclusions The HPLC-QAMS method can provide a accurate and feasible method with determination to establish multi-index component quality evaluation model for Runing granule.

关 键 词：高效液相一测多评法 乳宁颗粒 相对校正因子 多指标 质量控制 

分 类 号：R284.1[医药卫生—中药学]