超高效液相色谱法同时测定活血涤痰汤中7种活性成分的含量

Simultaneous determination of 7 active components in Huoxue Ditan decoction by UPLC

目的建立UPLC方法同时测定活血涤痰汤中黄芪甲苷、柴胡皂苷a、柴胡皂苷d、大黄酸、大黄素、大黄酚和大黄素甲醚含量。方法采用Waters BEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱,体积流量为0.3 mL·min^-1,进样量为3μL,检测波长分别为205和254 nm。结果黄芪甲苷、柴胡皂苷a、柴胡皂苷d、大黄酸、大黄素、大黄酚、大黄素甲醚的线性范围分别为2.89~57.76μg·m L^-1(r=0.9993)、2.10~42.08μg·m L^-1(r=0.9994)、3.04~60.88μg·m L^-1(r=0.9993)、1.06~21.12μg·m L^-1(r=0.9998)、0.89~17.84μg·m L^-1(r=0.9999)、1.18~23.60μg·m L^-1(r=0.9999)、1.14~22.88μg·m L^-1(r=0.9998),平均加样回收率分别为97.5%,97.3%、98.2%、99.3%、99.1%、99.1%和98.8%,RSD值分别为2.4%、2.5%、2.0%、2.0%、2.1%、2.1%和1.9%。结论建立的UPLC方法简便快速,重现性好,可用于活血涤痰汤的质量控制与评价。

Objective To establish a method to simultaneously determine astragalosideⅣ,saikosaponin a,saikosaponin d,rhein,emodin,chrysophanol and physcion in Huoxue Ditan decoction.Methods The determination was performed on a Waters BEH C18 column by gradient elution,with acetonitrile-0.1%phosphoric acid water solution as the mobile phase at the flow rate of 0.3 mL·min^-1.The injection volume was 3μL and the detection wavelength was 205 and 254 nm,respectively.Results AstragalosideⅣ,saikosaponin a,saikosaponin d,rhein,emodin,chrysophanol and physcion had a good linearity at 2.89-57.76μg·m L^-1(r=0.9993),2.10-42.08μg·m L^-1(r=0.9994),3.04-60.88μg·m L^-1(r=0.9993),1.06-21.12μg·m L^-1(r=0.9998),0.89-17.84μg·m L^-1(r=0.9999),1.18-23.60μg·m L^-1(r=0.9999),and 1.14-22.88μg·m L^-1(r=0.9998),respectively.The average recovery were 97.5%,97.3%,98.2%,99.3%,99.1%,99.1%and 98.8%,with RSDs of 2.4%,2.5%,2.0%,2.0%,2.1%,2.1%and 1.9%.Conclusion The UPLC method is simple,rapid and reproducible,which can be used for the quality control and evaluation of Huoxue Ditan decoction.