目的: 建立三七总皂苷中三七皂苷R1,人参皂苷Rg1、Re、Rb1和Rd的一测多评含量测定方法(QAMS),并验证其准确性。方法: 采用高效液相色谱法(HPLC),使用Welch PG C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-水为流动相,梯度洗脱,流速1.3 mL·min-1,柱温25 ℃,检测波长203 nm。分别采用标准曲线斜率法和浓度法测定,以人参皂苷Re为对照,分别计算其与三七皂苷R1,人参皂苷Rg1、Rb1和Rd的相对校正因子(RCFs),校正因子取2种方法的平均值,最终校正因子为3家省级以上食品药品监督检验研究院实验数据的平均值;采用一测多评法测定三七总皂苷中5个皂苷成分的含量。同时采用外标法测定三七总皂苷中5个皂苷成分的量,比较计算值与测定值之间的差异,验证一测多评法在测定中的准确性及可行性。结果: 以人参皂苷Re为对照,三七皂苷R1,人参皂苷Rg1、Re、Rb1和Rd的相对校正因子分别为0.996、0.856、1.000、1.165、0.996,20批样品QAMS计算的5个皂苷总量与外标法(ESM)测定结果之间的RSD均小于2.0%。结论: 本研究建立的三七总皂苷中5个皂苷含量测定的一测多评法重复性、准确性、耐用性良好,为三七总皂苷标准提高提供了依据。
Objective: To establish determination method for 5 saponins including notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd in notoginseng total saponins by quantitative analysis of multi components by single marker(QAMS). The accuracy of the method was validated. Methods: HPLC was performed on a Welch PG C18 column (250 mm×4.6 mm, 5 μm)withacetonitrile and water as the mobile phase with gradient elution at a flow of 1.3 mL·min-1. The column temperature was 25 ℃ and the detection wavelength was 203 nm. Ginsenoside Re was chosen as the reference substance, the relative correlation factors(RCFs)of notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1 and ginsenoside Rd were determined by standard curve slope method and concentration method, and the values of the correction factors were the average of the results of these two methods. The experiments of relative correction factors were repeated by NIFDC, Heilongjiang IFDC and Yunnan IFDC, and the final relative correction factor valueswerethe average of theexperimental data of three institutions. The content of five saponins in notoginseng total saponins was determined by multi-components by single marker(QAMS) method and external standard method (ESM). The QAMS method was validated through comparison of the results obtained by the two different methods. Results: The relative correlation factors of notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1 and ginsenoside Rd to ginsenoside Re were 0.996,0.856, 1.000, 1.165, 0.996 5, respectively. The RSD of the contents of 5 saponins determined by QAMS and ESM in 20 batches of notoginseng total saponinwerewas less than 2.0%. Conclusion: The established theQAMS method to the determination of five saponins in notoginseng total saponins has good repeatability, accuracy and durability. It provids a basis for the improvement of the standard for notoginseng total saponins.
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