HPLC-CAD同时测定保心宁片中3种皂苷含量

Simultaneous determination of three saponins in Baoxinning tablets by HPLC-CAD

目的:建立高效液相色谱-电雾式检测器(HPLC-CAD)方法同时测定保心宁片中3种皂苷的含量。方法:采用Thermofisher C18(5μm,4.6×250 mm)为色谱柱,乙腈(B)-水(A)为流动相进行梯度洗脱(0~5 min,18%B;5~45 min,18%→31%B;45~60 min,31%→45%),流速为1.0 mL·min^(-1),柱温为30℃,进样量为10μL。CAD检测器参数设置:雾化温度Low,数据采集频率10 Hz,滤波常数10 s。结果:三七皂苷R1、人参皂苷Rg1、Rb1分别在0.1338~1.3380 ug(r=0.9991)、0.4420~4.4200 ug(r=0.9997)、0.4040~4.0400 ug(r=0.9993)范围内线性关系良好,精密度、重复性、稳定性试验的RSD均小于3.0%,平均加样回收率分别为102.89%、102.35%、103.37%,RSD分别为1.10%、1.54%、1.58%(n=6)。结果表明该方法准确、简捷、可靠,可用于保心宁片中3种皂苷的含量测定。结论:建立了HPLC-CAD法同时测定保心宁片中3种皂苷的含量测定方法,对更好控制保心宁片质量具有重要的意义,同时该方法也可为其他含三七中成药中以上三种皂苷的含量测定研究做出参考。

Objective:To establish a high performance liquid chromatography-charged aerosol detector(HPLC-CAD)method to simultaneously detect the contents of three saponins in Baoxinning tablets.Method:Thermofisher C18 column(5μm,4.6×250 mm)was used.Acetonitrile(B)-water(A)was the mobile phase for gradient elution(0~5 min,18%B;5~45 min,18%→31%B;45→60 min,31%→45%)with the flow rate of 1.0 mL·min^(-1)at 30℃.The injection volume is 10μL.CAD detector parameter was as following:the atomization temperature was Low,the data acquisition frequency was 10 Hz,and the filter constant was 10 s.Result:Notoginsenoside R1,ginsenoside Rg1,and Rb1 had a good linear relationship within the range of 0.1338~1.3380μg(r=0.9991),0.4420~4.4200μg(r=0.9997),0.4040~4.0400μg(r=0.9993),respectively.The RSD of precision,repeatability,and stability tests were all less than 3.0%.The average sample recovery rates were 102.89%,102.35%,and 103.37%,with RSD of 1.10%,1.54%,and 1.58%,respectively(n=6).The results showed that the method was accurate,simple,and reliable,and can be used to detect the content of three saponins in Baoxinning tablets.Conclusion:The HPLC-CAD method has been established for the simultaneous determination of the content of 3 saponin in Baoxinning tablets,which is of great significance to better control the quality of Baoxinning tablets.At the same time,this method can also makes reference for other Chinese patent medicines containing Panax notoginseng.