高效液相色谱四级杆飞行时间串联质谱法测定启脾丸中7种人参皂苷的含量

Determination of 7 Kinds of Ginsenoside in Qipi Pills by HPLC-QTOF-MS

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 simultaneously determine the contents of ginsenoside RbI , ginsenoside Rb2, ginsenoside Rb3, ginsen- oside Re, ginsenoside Rg1 , ginsenoside Rf and ginsenoside Ro in Qipi pills by HPLC-QTOF-MS. Methods： The determination was performed on an Agilent Poroshell 120 EC-C18 column （2.1 mm × 50 mm,2.7 μm） with mobile phase consisting of acetonitrile（ A）- water（ B, containing 0.1% formic acid） with gradient elution. The flow rate was 0.21 ml min-1. The column temperature was 30 ℃. The MS instrument was equipped with an ESI＋ ion source. The exacted ion chromatograms were used to determine the quantities of different compounds in the samples while the mass spectra of product ions were used for confirming the compounds. Results ： All the 7 kinds of ginsenoside showed good linearity （ r 〉 0. 999 3 ）. The RSDs of precision, repeatability and stability tests were all less than 5%. The average recoveries were within the range of 97.11%-101. 98%. Conclusion： The method is simple, rapid and reliable with high specificity, which can be used for the quality control of Qipi pills.