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目的:建立高效液相色谱四级杆飞行时间串联质谱(HPLC-QTOF-MS)法,测定启脾丸中人参皂苷Rb_1、人参皂苷Rb_2、人参皂苷Rb_3、人参皂苷Re、人参皂苷Rg_1、人参皂苷Rf、人参皂苷Ro 7个成分含量的方法。方法:使用Agilent Poroshell 120 EC-C_(18)色谱柱(2.1 mm×50 mm,2.7μm);流速为0.21 ml·min~(-1);柱温为30℃;流动相为乙腈-水(含0.1%甲酸)系统梯度洗脱;采用电喷雾离子源(ESI),正离子方式检测,利用一级质谱的提取离子流色谱图进行定量,同时利用二级质谱进行成分的确认。结果:上述7种人参皂苷在一定范围内具有较好的线性关系,r值均大于0.999 3,精密度、重复性和稳定性的RSD都小于5%,加样回收率均在97.11%~101.98%之间。结论:本试验建立的方法简便、快速、可靠,经验证专属性较强,可为控制该制剂的质量提供依据。
Objective: To establish a HPLC-QTOF-MS method for the determination of ginsenoside Rb_1, ginsenoside Rb_2, ginsenoside Rb_3, ginsenoside Re, ginsenoside Rg_1, ginsenoside Rg_1, Rf, ginsenoside Ro content of seven components. Methods: The Agilent Poroshell 120 EC-C 18 column (2.1 mm × 50 mm, 2.7 μm) was used. The flow rate was 0.21 ml · min -1. The column temperature was 30 ℃. The mobile phase consisted of acetonitrile-water 0.1% formic acid). The electrospray ionization (ESI) and positive ion mode were used for the determination. The components were identified by ion-exchange chromatogram of the first-order mass spectrometry and the components were confirmed by the second-order mass spectrometry. Results: The above seven kinds of ginsenosides had a good linear relationship within a certain range, r values were greater than 0.999 3, the RSD of precision, repeatability and stability were less than 5%, and the recovery rates were 97.11% ~ 101.98 %between. Conclusion: The method established in this study is simple, rapid and reliable, and has strong specificity of verification. It can provide basis for controlling the quality of the preparation.