流速/溶剂双梯度反相高效液相色谱法快速同时测定复方丹参片中7种有效成分

采用整体柱建立了流速/溶剂双梯度反相高效液相色谱法快速同时测定复方丹参片中三七皂苷R1,人参皂苷Rg1,Re,Rb1,Rd,Rb2及丹参酮ⅡA 7种有效成分。通过对溶剂和流速双梯度体系的逐步优化,并应用色谱模拟软件Dry Lab,得到分离7种成分的最佳色谱条件。采用色谱柱Merck Chromolith Performance RP-18e(100 mm×4.6 mm),以乙腈-水为流动相体系,流速/溶剂双梯度洗脱,柱温30℃;片剂中的7种成分在21 min内达到基线分离;Rg1在60.60~242.40 mg/L(r=0.999 0)、丹参酮ⅡA在16.52~66.08 mg/L(r=0.999 9),其余皂苷在30.70~142.66 mg/L(r≥0.999 4)范围内具有良好的线性关系;定量下限(S/N=10)为21~124μg/kg,回收率为96.7%~100.1%。该方法能在短时间内同时分离不同极性的化合物,提高被测物的柱效,减少半峰宽和拖尾,可应用于复方丹参片中7种成分的含量分析。

Rapid and Simultaneous Determination of Seven Active Components in Compound Salvia Miltiorrhiza Bunge Tablets by Flow Rate/Organic Solvent Double-gradient High Performance Liquid Chromatography

A flow rate/organic solvent double-gradient mode in reversed-phase high performance liquid chromatography (HPLC) by using monolithic column was established as a new approach for the rapid and simultaneous determination of notoginsenoide R1,ginsenosides Rg1,Re,Rb1,Rd,Rb2 and tanshinone Ⅱ A in compound Salvia miltiorrhiza bunge tablets.Through the optimization of the flow rate/organic solvent double-gradient mode,and combination with chromatographic simulation software DryLab,the optimized double-gradient HPLC system for the seven active components was built.The determination was carried out on a Merck Chromolith Performance RP-18e(100 mm× 4.6 mm) column using acetonitrile-water as mobile phase at a column temperature of 30 ℃.The separation of seven active components in the tablets was achieved in 21 min.The linear ranges were 60.60-242.40 mg/L(r =0.999 0) for Rg1,16.52-66.08 mg/L(r =0.999 9) for tanshinone Ⅱ A,and 30.70-142.66 mg/L(r≥0.999 4) for the other active components.The LOQs(S/N=10) were in the range of 21-124 μg/kg and the mean recoveries were 96.7％-100.1％.The method could be used for the simultaneous determination of different polarity compounds in a short time.It also could improve the column efficiency of the analytes,compress the half-peak width and reduce the trailing.Therefore,the method could be used for the rapid and simultaneous determination of the seven active components in compound Salvia miltiorrhiza bunge tablets.