波长切换-超高效液相色谱法检测女珍颗粒中特女贞苷、蟛蜞菊内酯和β,β'-二甲基丙烯酰阿卡宁的含量

Determination of nuezhenide,wedelolactone andβ,β'-dimethylacryloyl akanin in Nüzhen Granules by wavelength switching and UPLC

目的建立检测女珍颗粒中特女贞苷、蟛蜞菊内酯和β,β'-二甲基丙烯酰阿卡宁含量的波长切换-超高效液相色谱法(UPLC)。方法色谱柱:Agilent Eclipe SB C_(18)液相色谱柱;检测波长:225 nm(特女贞苷)、352 nm(蟛蜞菊内酯)、276 nm(β,β'-二甲基丙烯酰阿卡宁);柱温:30℃;流速:1.0 mL·min^(-1);进样量:10μL;流动相:5mL·L^(-1)冰醋酸溶液(A)-乙腈(B);梯度洗脱。用外标法定量检测。结果特女贞苷、蟛蜞菊内酯和β,β'-二甲基丙烯酰阿卡宁质量浓度分别在0.475~47.5、0.0972~9.72、0.196~19.6μg·mL^(-1)范围内与其峰面积线性关系良好;加标回收率分别为98.8%、99.3%、100.4%;重复性RSD值(n=6)分别为1.2%、0.91%、1.3%。结论建立的方法具有快速、准确等特点,可用于女珍颗粒中成药的质量控制,为其测定标准的提高提供技术参考。

Objective To establish wavelength switching and ulltra-performance liquid chromatography(UPLC)method for the determination of nuezhenide,wedelolactone and β,β'-dimethylacryloyl akanin in Nüzhen Granules.Methods Agilent Eclipe SB C_(18) was used for separation,the detection wavelength was set at 225 nm(nuezhenide),352 nm(wedelolactone)and 276 nm(β,β'-dimethylacryloyl akanin)with column temperature was 32℃,flow rate was 1.0 mL·min^(-1),injection volume was 10μL.The mobile phase A was 5mL·L^(-1) glacial acetic acid and mobile phase B was acetonitrile in a gradient elution mode.External standard method was selected for the quantitation.Results Nuezhenide,wedelolactone and β,β'-dimethylacryloyl akanin showed good linear relationships with their peak areas at the mass concentrations of 0.475-47.5,0.0972-9.72,and 0.196-19.6μg·mL^(-1),respectively.The average recoveries were 98.8%,99.3% and 100.4%,respectively.The relative standard deviation(RSD)of repeatability test were 1.2%,0.91% and 1.3%(n=6),respectively.Conclusion The results showed that this method is rapid and accurate,and can be used for the quality control of Nüzhen Granules.The study also provides a technical reference for improving the measuvement standards.