高效液相色谱波长切换法同时测定归芍调经片中9种成分的含量

Simultaneous determination of 9 components in Guishao Tiaojing tablets by HPLC wavelength switching method

目的建立HPLC波长切换法同时测定归芍调经片中9种活性成分的含量。方法采用Waters XBridge-C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈(A)-0.05%磷酸溶液(B),梯度洗脱;检测波长:232 nm(芍药内酯苷和芍药苷)、208 nm(柴胡皂苷a、柴胡皂苷d和23-乙酰泽泻醇B)、220 nm(白术内酯Ⅲ、白术内酯Ⅰ和茯苓酸)、278 nm(白术内酯Ⅱ),流速:0.8 mL·min^(-1),柱温:30℃,进样量:10μL。结果芍药内酯苷、芍药苷、柴胡皂苷a、柴胡皂苷d、23-乙酰泽泻醇B、白术内酯Ⅲ、白术内酯Ⅰ、茯苓酸、白术内酯Ⅱ分别在6.088~121.760、17.640~352.088、1.010~20.192、0.406~8.112、0.106~2.118、3.216~64.320、3.008~60.160、4.072~81.440、2.232~44.640μg·mL^(-1)(r为0.9995~0.9998)内与峰面积呈良好的线性关系;平均加样回收率分别为97.1%、99.7%、97.4%、98.0%、96.6%、101.0%、98.5%、98.6%、95.5%,RSD(n=6)分别为0.5%、0.6%、1.5%、0.8%、1.1%、0.8%、0.7%、0.4%、1.0%。结论本方法可为归芍调经片的质量控制提供依据。

Objective To establish an HPLC wavelength switching method to determine 9 active components in Guishao Tiaojing tablets simultaneously.Methods A Waters XBridge-C18 column(250 mm×4.6 mm,5μm)was used.The mobile phase consisted of acetonitrile(A)-0.05%aqueous phosphoric acid(B)with gradient mode at the flow rate of 0.8 mL·min^(-1).The detection wavelength was 232 nm for albiflorin and paeoniflorin,208 nm for saikosaponin a,saikosaponin d and 23-acetate alisol B,220 nm for atractylenolideⅢ,atractylenolideⅠand pachymic acid,and 278 nm for atractylenolideⅡ.The column temperature was 30℃and the injection volume was 10μL.Results The linearity of albiflorin,paeoniflorin,saikosaponin a,saikosaponin d,23-acetate alisol B,atractylenolideⅢ,atractylenolideⅠ,pachymic acid,and atractylenolideⅡwas 6.088~121.760,17.640~352.088,1.010~20.192,0.406~8.112,0.106~2.118,3.216~64.320,3.008~60.160,4.072~81.440,and 2.232~44.640μg·mL^(-1)(r=0.9995~0.9998).The average recovery was 97.1%,99.7%,97.4%,98.0%,96.6%,101.0%,98.5%,98.6%,and 95.5%with RSD(n=6)at 0.5%,0.6%,1.5%,0.8%,1.1%,0.8%,0.7%,0.4%,and 1.0%.Conclusion The HPLC wavelength switching method for the simultaneous determination of 9 components can be used to control the quality of Guishao Tiaojing tablets.