[关键词]
[摘要]
目的 建立熟三七粉的HPLC特征图谱,并对其8种稀有皂苷的含量进行测定,结合偏最小二乘法判别分析(PLS-DA)和聚类分析,为熟三七粉质量的科学评价提供方法。方法 采用Agilent Zorbax SB-C18(250 mm×4.6 mm,5 μm)色谱柱,以乙腈(A)-水(B)为流动相洗脱梯度:0~10 min,19%~33% A;10~30 min,33%~38% A;30~45 min,38%~50% A;45~60 min,50%~60% A,体积流量1.0 mL/min,检测波长203 nm,柱温40℃,进样量10 μL,建立熟三七粉的HPLC特征图谱,并对其人参皂苷20(S)-Rh1、20(R)-Rh1、Rk3、Rh4、20(S)-Rg3、20(R)-Rg3、Rk1和Rg5共8种指标性成分定量测定方法进行方法学考察,对63批熟三七粉进行含量测定。结果 建立了熟三七粉的HPLC特征图谱,共标定19个共有峰。同时测定8种稀有皂苷成分含量,色谱峰达到了较好的分离,且线性关系良好,8种皂苷线性回归方程的相关系数分别为0.999 9、0.999 5、0.999 4、0.999 3、0.999 1、0.999 3、0.999 1、0.999 3;平均加样回收率为95%~105%;RSD值均低于2%。63批样品按色泽分为棕红色与淡黄色2组,棕红色组质量明显优于淡黄色组。结论 熟三七粉的质量优劣与色泽有关,该方法灵敏、准确、重现性好,可为熟三七粉的质量评价提供参考。
[Key word]
[Abstract]
Objective To establish the method for the specific chromatograms analysis of steamed Panax notoginseng Powder and determine the content of eight components, combined with clustering analysis and partial least square discriminant analysis (PLS-DA), with aim to provide reference for the quality control of steamed Panax notoginseng Powder. Methods HPLC with Agilent ZORBAX SB-C18 column (250 mm×4.6 mm, 5 μm) was used, the mobile phase was acetonitrile (B)-water (A) in a gradient elution mode, the detection wavelength was set at 203 nm, the flow rate was 1.0 mL/min, the column temperature was 40℃, and sample size 10 ìL. HPLC characteristic spectrum of steamed Panax notoginseng Powder was established, and quantitative determination methods of eight index components, ginsenoside 20 (S)-Rh1, 20 (R)-Rh1, Rk3, Rh4, 20 (S)-Rg3, 20 (R)-Rg3, Rk1 and Rg5, were investigated, its content in 63 batches of samples were determined. Results The specific chromatograms of steamed Panax notoginseng Powder effective parts were established and 19 common peaks were designated. Among them, eight rare saponins including ginsenoside 20 (S)-Rh1, 20 (R)-Rh1, Rk3, Rh4, 20 (S)-Rg3, 20 (R)-Rg3, Rk1 and Rg5 all showed good linear relationship within the ranges of 0.999 9, 0.999 5, 0.999 4, 0.999 3, 0.999 1, 0.999 3, 0.999 1, and 0.999 3, respectively. The average recovery was 95%-105%, with the RSD value less than 2%. Moreover, the 63 batches of samples were divided into two groups:brown red and light yellow, and the quality of brown red group was obviously better than that of pale yellow group. Conclusion The quality of the steamed Panax notoginseng Powder is related to the color and lustre. This method is accurate, sensitive and reproducible, which can provide reference for the quality evaluation of steamed Panax notoginseng Powder.
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[基金项目]
国家中药标准化项目:三七等2种中药饮片标准化建设(ZYBZH-Y-YN-44)