基于HPLC-QAMS法同时测定清肺散结丸中阿克苷、苦玄参苷ⅠB、苦玄参苷ⅠA、三七皂苷R1、绞股蓝皂苷XLⅨ、绞股蓝皂苷A和绞股蓝皂苷ⅩⅦ的含量

Determination of Verbascoside,Picfeltarraenin ⅠB,Picfeltarraenin ⅠA,Notoginsenoside R,Gypenoside XLⅨ,Gypenoside A and Gypenoside ⅩⅦ in Qingfei Sanjie Pills by HPLC-QAMS

目的:建立高效液相一测多评法同时测定清肺散结丸中阿克苷、苦玄参苷ⅠB、苦玄参苷ⅠA、三七皂苷R1、绞股蓝皂苷ⅩLⅨ、绞股蓝皂苷A和绞股蓝皂苷ⅩⅦ的含量。方法:采用高效液相一测多评法,以Welch Material C18(250 mm×4.6 mm,5μm)为色谱柱,柱温:25℃;流动相为乙腈-0.2%冰醋酸水溶液,梯度洗脱,流速为0.9 ml·min-1;检测波长分别为264 nm(检测阿克苷、苦玄参苷ⅠB和苦玄参苷ⅠA)和203 nm(检测三七皂苷R1、绞股蓝皂苷XLⅨ、绞股蓝皂苷A和绞股蓝皂苷ⅩⅦ)。以苦玄参苷ⅠA为内参物,建立其与阿克苷、苦玄参苷ⅠB、三七皂苷R1、绞股蓝皂苷XLⅨ、绞股蓝皂苷A和绞股蓝皂苷ⅩⅦ的相对校正因子,计算各成分含量。结果:阿克苷、苦玄参苷ⅠB、苦玄参苷ⅠA、三七皂苷R1、绞股蓝皂苷XLⅨ、绞股蓝皂苷A和绞股蓝皂苷ⅩⅦ分别在1.87~46.75μg·ml-1(r=0.9991)、2.03~50.75μg·ml-1(r=0.9997)、1.06~26.50μg·ml-1(r=0.9993)、0.97~24.25μg·ml-1(r=0.9996)、0.81~20.25μg·ml-1(r=0.9991)、1.39~34.75μg·ml-1(r=0.9997)、2.26~56.50μg·ml-1(r=0.9995)范围内线性关系良好;平均加样回收率(RSD)分别为98.83%(0.97%),100.11%(0.62%),97.92%(1.38%),96.96%(1.40%),97.74%(1.18%),99.15%(0.89%)和99.36%(1.01%)(n=9);一测多评法的计算值与外标法(ESM)测定值间无明显差异。结论:所建立的HPLC-QAMS法结果准确,可用于清肺散结丸的质量控制。

Objective: To develop an HPLC-QAMS method for the simultaneous determination of verbascoside,picfeltarraeninⅠB,picfeltarraenin ⅠA,notoginsenoside R1,gypenoside XLⅨ,gypenoside A and gypenoside ⅩⅦ in Qingfeisanjie pills. Methods:An HPLC method with a Welch Material C18( 250 mm×4.6 mm,5 μm) column was applied,the mobile phase was acetonitrile-0.2%glacial acetic acid aqueous solution,the flow rate was 0.9 ml·min-1,and the column temperature was 25 ℃.The detection wavelengths were set at 264 nm for verbascoside,picfeltarraenin ⅠB and picfeltarraenin ⅠA,and 203 nm for notoginsenoside R1,gypenoside XLⅨ,gypenoside A and gypenoside ⅩⅦ. Using picfeltarraenin ⅠA as an internal standard,the relative correction factors of verbascoside,picfeltarraenin ⅠB,notoginsenoside R1,gypenoside XLⅨ,gypenoside A and gypenoside ⅩⅦ were obtained,and the content of each component was calculated. Results: Verbascoside,picfeltarraenin Ⅰ B,picfeltarraenin Ⅰ A,notoginsenoside R1,gypenoside XLⅨ,gypenoside A and gypenoside ⅩⅦ showed good linear relationship within the range of 1.87-46.75 μg·ml-1( r =0.999 1),2.03-50.75 μg·ml-1( r= 0.999 7),1.06-26.50 μg·ml-1( r = 0.999 3),0.97-24.25 μg·ml-1( r = 0.999 6),0.81-20.25μg·ml-1( r= 0.999 1),1.39-34.75 μg·ml-1( r= 0.999 7) and 2.26-56.50 μg·ml-1( r = 0.999 5),respectively,the average recovery and RSDs were 98.83%( 0.97%),100.11%( 0.62%),97.92%( 1.38%),96.96%( 1.40%),97.74%( 1.18%),99.15%( 0.89%) and 99.36%( 1.01%)( n= 9),respectively. There were no statistical differences between the calculated values by QAMS and the measured ones by ESM. Conclusion: The established HPLC-QAMS method is accurate,and can be used for the quality control of Qingfei Sanjie pills.