HPLC-DAD-ELSD法同步测定冠心丹参片中8个成分含量

Simultaneous determination of the contents of eight components in Guanxin Danshen Tablets by HPLC-DAD-ELSD

目的建立同时测定冠心丹参片中丹参素钠、原儿茶醛、丹酚酸B、丹参酮ⅡA、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1含量的方法。方法采用高效液相色谱-二极管阵列检测-蒸发光散射检测(HPLC-DAD-ELSD)法,色谱柱为Thermo Hypersil-Keystone C18(4.6 mm×250 mm,5μm);流动相为乙腈-0.03 mol/L醋酸铵(含甲酸,pH2.4),梯度洗脱;流速1.0 ml/min;柱温25℃,DAD检测波长280 nm,进样量20μl,ELSD设定参数:漂移管温度113℃,载气流速3.1 L/min。结果丹参素钠、原儿茶醛、丹酚酸B、丹参酮ⅡA、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1分别在进样量3.0750~18.4500、0.0400~0.2400、0.8000~4.8000、0.0605~0.3630、0.7160~4.2960、0.1056~0.6333、0.6055~3.6330、0.6975~4.1850μg范围内与色谱峰面积线性关系良好,r均在0.9964~0.9998范围之内,加样回收率(n=6)分别为101.70%、96.85%、104.2%、99.63%、102.60%、100.80%、99.71%、101.20%,RSD分别为1.88%、3.13%、1.93%、1.41%、1.71%、1.88%、3.24%、2.11%。结论所建立的测定方法具较好的专属性、精密度、重复性和稳定性,适用于冠心丹参片中8个成分的测定,可为完善冠心丹参片质量控制提供参考。

Objective To establish an method for the simultaneous determination of the contents of Sodium salvianolic acid,protocatechualdehyde,salvianolic acid B,tanshinoneⅡA,Panax notoginseng saponin R1,ginsenoside Rg1,ginsenoside Re,and ginsenoside Rb1 in Guanxin Danshen Tablets.Method HPLC-DAD-ELSD method was used,and the chromatographic column was Thermo Hypersil Keystone C18 column(4.6 mm×250 mm,5μm);mobile phase was acetonitrile(A)-0.03 mol/L ammonium acetate(containing formic acid,pH 2.4)(B),gradient elution;flow rate was 1.0 ml/min;column temperature was 25℃,and DAD detection wavelength was 280 nm,and injection amount was 20μl.ELSD setting parameters:drift tube temperature:113℃,carrier gas flow rate:3.1 L/min.Results Sodium salvianolic acid,protocatechualdehyde,salvianolic acid B,tanshinoneⅡA,Panax notoginseng saponin R1,ginsenoside Rg1,ginsenoside Re,and ginsenoside Rb1 were tested at injection rates of 3.0750-18.4500,0.0400-0.2400,0.8000-4.8000,0.0605-0.3630,0.7160-4.2960,0.1056-0.6330,0.6055-3.6330,0.6975-4.1850μg,respectively.The linear relationship between the peak area and the g range was good,with r all within the range of 0.9964 to 0.9998.The recovery rates(n=6)of the added samples were 101.70%,96.85%,104.20%,99.63%,102.60%,100.80%,99.71%,and 101.20%,respectively.The RSDs were 1.88%,3.13%,1.93%,1.41%,1.71%,1.88%,3.24%,and 2.11%,respectively.Conclusion The determination method established in this article has good specificity,precision,repeatability,and stability,and is suitable for the determination of 8 components in Guanxin Danshen Tablets,providing reference for improving the quality control of Guanxin Danshen Tablets.