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目的建立高效液相色谱串联质谱法测定知柏地黄浓缩丸中新芒果苷,芒果苷,知母皂苷BⅡ,知母皂苷AⅢ,小檗碱,莫诺苷,马钱苷,芍药苷和丹皮酚含量的方法。方法采用Diamonsil C18柱(4.6 mm×150 mm,5μm);柱温30℃;乙腈-0.1%甲酸水溶液为流动相,以800μL·min-1梯度洗脱;质谱条件:采用电喷雾离子源正负离子模式同时进行检测,多反应监测模式(MRM)用于定量测定。结果知柏地黄丸中9种成分峰面积与浓度呈良好的线性关系,在15 min内知柏地黄丸中9种成分峰面积与浓度线性关系良好,r>0.999 3;加样回收率(n=3)分别为98.33%,99.73%,100.1%,101.2%,101.2%,100.2%,99.90%,100.6%和100.5%。RSD值分别为1.99%,1.57%,1.21%,2.73%,1.76%,1.59%,1.11%,1.70%和1.05%。结论该方法简便,准确,重现性好,专属性高,可用于知柏地黄丸的质量控制。
OBJECTIVE To establish a HPLC-MS / MS method for the determination of neogenin, mangiferin, timosaponin BⅡ, timosaponin A Ⅲ, berberine, morroniside, loganin, paeoniflorin and paeoniflorin Method of phenol content. Methods Diamonsil C18 column (4.6 mm × 150 mm, 5 μm) was used. The column temperature was 30 ℃. Acetonitrile-0.1% formic acid aqueous solution was used as the mobile phase and the gradient was 800 μL · min-1. Mass spectrometry conditions: electrospray ionization Mode simultaneous detection, multiple reaction monitoring mode (MRM) for quantitative determination. Results There was a good linear relationship between the peak areas and the concentrations of nine components in Zhibai Dihuang Wan. The linear relationship between the peak area and the concentration of nine components in Zhibaihuanghuang Pills was good within 15 min (r> 0.999 3). The recoveries (n = 3) were 98.33%, 99.73%, 100.1%, 101.2%, 101.2%, 100.2%, 99.90%, 100.6% and 100.5%, respectively. RSD values were 1.99%, 1.57%, 1.21%, 2.73%, 1.76%, 1.59%, 1.11%, 1.70% and 1.05%, respectively. Conclusion The method is simple, accurate, reproducible and highly specific and can be used for quality control of Zhibi Di Huang Wan.