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目的:建立HPLC-ELSD法测定特制接骨丸中三七皂苷R_1、人参皂苷Rg_1和人参皂苷Re3种皂苷含量的分析方法。方法:采用HPLC-ELSD法,色谱柱为Wonda Sil C_(18)柱(4.6 mm×250 mm,5μm);流动相:乙腈(A)-水(B),梯度洗脱(0~10 min,19%→21%A;10~19 min,21%→23%A;19 min~20 min,23%→32%A;20~28 min,32%A;28~29 min,32%→33%A;29~40 min,33%A;40~41 min,33%→19%A;41~48 min,19%A);柱温:25℃;流速:1.0m L·min~(-1);ELSD检测器参数:漂移管温度为108℃,气体流量为2.8 L·min~(-1)。结果:三七皂苷R_1、人参皂苷Rg_1、人参皂苷Re分别在进样量为0.515~1.030、2.500~5.000、1.510~3.020μg线性关系良好,三七皂苷R_1、人参皂苷Rg_1、人参皂苷Re平均加样回收率分别为99.67%、97.49%、101.74%。结论:HPLC-ELSD法可以准确、快速地实现特制接骨丸中多种皂苷类成分的定量测定,从而用于特制接骨丸的质量控制。
OBJECTIVE: To establish a HPLC-ELSD method for the determination of saponins of Panax notoginseng saponins R_1, ginsenosides Rg_1 and ginsenosides Re. Methods: The mobile phase consisted of acetonitrile (A) - water (B) and gradient elution (0 ~ 10 min, gradient elution was performed on a Wonda Sil C 18 column (4.6 mm × 250 mm, 19% → 21% A; 10-19 min, 21% → 23% A; 19-20 min, 23% → 32% A; 20-28 min, 32% A; % A; 29-40 min 33% A; 40-41 min 33% 19% A 41-48 min 19% A); column temperature 25 ° C .; flow rate 1.0 mL · min -1 1); ELSD detector parameters: the drift tube temperature is 108 ℃, the gas flow rate is 2.8 L · min ~ (-1). Results: The calibration curves of notoginsenoside R_1, ginsenoside Rg_1 and ginsenoside Re were good at 0.515 ~ 1.030, 2.500 ~ 5.000 and 1.510 ~ 3.020μg injection volume respectively. The average concentrations of notoginsenoside R_1, ginsenoside Rg_1 and ginsenoside Re The recovery rates were 99.67%, 97.49% and 101.74% respectively. Conclusion: The HPLC-ELSD method can accurately and quickly achieve the quantitative determination of various saponin components in the special jigao pill and thus can be used for the quality control of the special jigao pill.