超高效液相色谱法快速测定血栓通注射液中5种皂苷成分的含量

A rapid method for the simultaneous determination of five saponins in Xueshuantong injection with ultra performance liquid chromatography

目的:建立一种快速测定血栓通注射液中皂苷成分含量的方法,为优化产品质量摔制方法提供参考。方法:应用新型的超高效液相色谱系统,使用1.7μm填料的 BEH C_(18)色谱柱(50 mm×2.1mm),乙腈(A)-水(B)两相溶剂梯度洗脱[0～5.5min,18%A→19%A;5.5～6.0min,19%A→31%A;6.0～9.5min,31%A→35%A],流速0.35 mL·min^(-1),紫外203 nm 下检测。结果:三七皂苷 R_1及人参皂苷 Rg_1、Re、Rb_1、Rd 在9.5 min 内即达到良好分离,在测定的浓度范围内线性关系良好(r>0.9984),日间及日内精密度的 RSD 均小于3.1%,最低定量限和最低检测限可分别达到0.5 ng 和0.2ng,半均回收率均大于95.0%。结论:超高效液相色谱法可同时测定血栓通注射液中5种皂苷成分,提高了分析效率,是一种快速可靠的质量控制手段。

Objective：To develop a rapid method for simultaneous determination of five saponins in Xueshuantong injection for optimization method of its quality control. Methods：The analysis was performed on ultra performance liquid chromatography（UPLC） system with BEH C18 column （50 mm× 2. 1 mm） filled with 1.7 μm particle, the gradient elution[0 -5.5 min, 18% A→19% A;5.5 - 6.0 min, 19% A→31% A;6. 0 - 9. 5 rain,31% A→35% A ] of acetonitrile（A） and water（B） were used for the separation at the flow rate of 0. 35 mL· min^-1, the samples were determined at 203 nm. Results： The five saponins namely notoginsenoside R1, ginsenoside Rg1, Re, Rb1 and Rd in Xueshuantong injection were well separated in 9.5 min. The results showed a good linearity（ r 〉0. 9984） within the test ranges. The overall intra - and inter - day variations（RSDs） of five saponins were less than 3.1%. And the LOQ and LOD were lower to 0. 5 ng and 0. 2 ng,respectively. The average recovery was more than 95.0%. Conclusion：It is a rapid and accurate method for quality evaluation of Xueshuantong injection.