UPLC-Q/TOF-MS法同时测定竹节参及其总皂苷中13个指标成分

Determination of 13 Components in Panacis Japonici Rhizoma and Its Total Saponins by UPLC-Q/TOF-MS

目的 建立测定竹节参及其总皂苷中人参皂苷Re、人参皂苷Rg1、人参皂苷Rf、人参皂苷Rg2、人参皂苷Rh1、人参皂苷Rb1、竹节参皂苷V、人参皂苷Rb2、拟人参皂苷RT1、人参皂苷Rb3、竹节参皂苷IV、竹节参皂苷IVa、人参皂苷Rd含量的超高效液相色谱-四级杆-飞行时间质谱法(UPLC-Q/TOF-MS),用以控制药材的质量。方法采用Waters UPLC HSS T3色谱柱(100 mm×2.1 mm, 1.8μm),乙腈(A)-0.1%甲酸水(B)梯度洗脱,流速0.4 mL/min, Waters Xevo G2 Q-Tof质谱仪,ESI负离子模式采集数据,采用一级质谱定量。结果 13个成分在相应的浓度范围内线性关系良好,相关系数均大于0.999 0,精密度、重复性、稳定性良好,平均加样回收率97.27%~100.86%,RSD<2.99%。13种成分在9批次竹节参药材中的含量依次为0.70~7.71、0.77~10.77、0.07~1.23、0.06~1.08、0.01~2.97、0.75~5.04、43.99~95.06、0.02~0.08、0.49~27.86、0.05~0.22、18.74~61.40、2.40~30.83、0.03~1.74 mg/g,在竹节参总皂苷中的含量依次为37.93、28.63、5.87、2.43、0.83、26.27、363.14、0.39、5.91、1.50、238.25、51.56、11.24 mg/g。结论 所建立的UPLC-Q/TOF-MS法可用于竹节参药材及总皂苷的指标成分的快速测定与质量评价。

Objective To establish an UPLC-Q/TOF-MS method for the determination of ginsenoside Re, ginsenoside Rg1,ginsenoside Rf, ginsenoside Rg2,ginsenoside Rh1,ginsenoside Rb1,chikusetsusaponin V,ginsenoside Rb2,pseudoginsenoside RT1,ginsenoside Rb3,chikusetsusaponin IV,chikusetsusaponin IVa, ginsenoside Rd in Panacis Japonici Rhizoma and its total saponins.Methods Data were collected using Waters UPLC HSS T3 column(100 mm×2.1 mm, 1.8 μm),acetonitrile(A)-0.1% formic acid in water(B) gradient elution, flow rate 0.4 mL/min, Waters Xevo G2 Q-Tof mass spectrometer, ESI negative ion mode, and quantified by first-order mass spectrometry.Results The 13 components showed good linear relationship(r~2>0.999 0) in the corresponding concentration range.The precision, repeatability and stability are good and the average sample recovery rate is 97.27%~100.86%(RSD<2.99%).The contents of 13 components in 9 batches of Panax Japonicas Rhizoma were 0.70~7.71,0.77~10.77,0.07~1.23,0.06~1.08,0.01~2.97,0.75~5.04,43.99~95.06,0.02~0.08,0.49~27.86,0.05~0.22,18.74~61.40,2.40~30.83 and 0.03~1.74 mg/g, and in total saponins were 37.93,28.63,5.87,2.43,0.83,26.27,363.14,0.39,5.91,1.50,238.25,51.56 and 11.24 mg/g.Conclusion This UPLC-Q/TOF-MS method can be used for rapid determination and quality evaluation of Panacis Japonici Rhizoma and its total saponins.