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目的建立用于测定注射用益气复脉(冻干)(YFI)中9种成分人参皂苷Rb_1(Rb_1)、Rg_1(Rg_1)、Re(Re)、Rf(Rf)、Rc(Rc)、Ro(Ro)、Rb_2(Rb_2)、Rd(Rd)及五味子醇甲(Sch)的一测多评(QAMS)方法,探讨QAMS法用于不同类型化学成分定量测定的准确性与可行性。方法采用高效液相色谱法,Diamonsil~?C_(18)(2)(250 mm×4.6 mm,5μm)色谱柱,乙腈-0.05%磷酸水溶液为流动相,梯度洗脱,柱温30℃,体积流量为1 m L/min,检测波长203 nm。建立Rg_1、Re、Rf、Rc、Ro、Rb_2、Rd及Sch与内参物Rb_1的相对校正因子(f),通过f计算YFI中8种成分的量,并在25批YFI中进行验证,将该方法与外标法测定的结果进行对比分析,以验证QAMS法的合理性、可行性和可重复性。结果 Rg_1、Re、Rf、Rb_1、Rc、Ro、Rb_2、Rd、Sch分别在进样量为0.929~4.644、0.818~4.089、0.732~3.660、1.461~7.305、0.636~3.181、0.618~3.092、0.788~3.941、0.758~3.789、0.178~0.889μg线性关系良好,加样回收率为97.08%~100.94%;f值分别为f_(Rg_1/Rb_1)=1.970,f_(Re/Rb_1)=0.929,f_(Rf/Rb_1)=1.196,f_(Rc/Rb_1)=0.870,f_(Ro/Rb_1)=0.830,f_(Rb_2/Rb_1)=0.786,f_(Rd/Rb_1)=0.906,f_(Sch/Rb_1)=12.082,且在不同条件下重复性良好;QAMS法的计算结果与外标法的实测值之间无显著性差异,实验所得的f值可信。结论本实验建立的QAMS法可以作为一种简便准确的质量评价模式用于YFI中多种人参皂苷类成分和Sch的质量控制。
OBJECTIVE To establish a method for the determination of 9 components of Rb_1, Rg_1, Re (Re), Rf (Rf), Rc (Rc), Ro Roam, Rb_2, Rd (Rd), and Schisandra chinensis (Sch) to investigate the accuracy and feasibility of the QAMS method for the quantitative determination of different types of chemical constituents. Methods High performance liquid chromatography (HPLC) was performed on a Diamonsil C 18 column (250 mm × 4.6 mm, 5 μm) column using acetonitrile-0.05% phosphoric acid as mobile phase with gradient elution at 30 ℃. The flow rate was 1 m L / min and the detection wavelength was 203 nm. The relative correction factors (f) of Rg_1, Re, Rf, Rc, Ro, Rb_2, Rd and Sch and the reference substance Rb_1 were established. The quantities of the eight components in YFI were calculated by f and validated in 25 batches of YFI. Methods and external standard method to determine the results of comparative analysis to verify the QAMS method rationality, feasibility and repeatability. Results Rg_1, Re, Rf, Rb_1, Rc, Ro, Rb_2, Rd and Sch were respectively measured at injection rates of 0.929-4.464, 0.818-4.08, 0.732-3.660, 1.461-7.305, 0.636-3.181, 0.618-3.092, 3.941,0.758 ~ 3.789,0.178 ~ 0.889μg, and the recoveries were 97.08% ~ 100.94%. The f values were respectively f_ (Rg_1 / Rb_1) = 1.970, f_ (Re / Rb_1) = 0.929, f_ /Rb_1)=1.196,f_(Rc/Rb_1)=0.870,f_(Ro/Rb_1)=0.830,f_(Rb_2/Rb_1)=0.786,f_(Rd/Rb_1)=0.906,f_(Sch/Rb_1)=12.082 , And the repeatability is good under different conditions. There is no significant difference between the calculated results of QAMS method and the measured values of the external standard method, and the f value obtained in the experiment is credible. Conclusion The QAMS method established in this experiment can be used as a simple and accurate quality evaluation model for the quality control of various ginsenosides and Sch’s in YFI.