山楂降脂软胶囊中4种黄酮含量的测定*
Simultaneous quantification of four flavonoids in hawthorn lipid-lowering soft capsules

目的:建立同时测定山楂降脂软胶囊中4种主要黄酮葛根素、木犀草素、槲皮素及儿茶素的超高效液相-串联质谱法。方法:在超声条件下用甲醇提取山楂降脂软胶囊供试品。采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7 μm)色谱柱分离,以体积分数0.1%甲酸乙腈和体积分数0.1%甲酸水溶液为流动相梯度洗脱,在负离子模式下采用多反应监测。结果:葛根素、木犀草素、槲皮素、儿茶素分别在0.03～8.10、0.04～8.27、0.02～4.45及0.01～3.11 mg/L的范围内线性良好,R2均＞0.992,4种黄酮的平均加样回收率在93.6%～107.5%,相对标准偏差在1.62%～2.21%。结论:建立了适用于快速测定山楂降脂软胶囊中4种黄酮的液质联用定量方法,该方法灵敏、准确、稳定,可用于山楂降脂软胶囊的质量控制。
Aim: To develop a quantitative method for simultaneous determination of puerarin, mignonette, quercetin and catechin in hawthorn lipid-lowering soft capsules using ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry.Methods: Hawthorn lipid-lowering soft capsules were extracted with methanol under the condition of ultrasound. The separation was carried out on a Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7 μm)column. And the mobile phase was consisted of acetonitrile-0.1%(V/V)formic acid and H2O-0.1%(V/V)formic acid in a gradient elution mode. Then the sample solution was analyzed in electrospray ionization-ion mode with multiple reaction monitoring.Results: The results suggested that puerarin, mignonette, quercetin and catechin exhibited a good linearity in the range of 0.03～8.10,0.04～8.27,0.02～4.45 and 0.01～3.11 mg/L, respectively. And the correlation coefficient was higher than 0.992. The average recovery rate of the 4 flavonoids was in the range of 93.6%～107.5%, while the range of relative standard deviation was 1.62%～2.21%.Conclusion: The established method is sensitive, accurate and stable, and meet the requirement for determination of the 4 major flavonoids in hawthorn lipid-loweringsoft capsules, thus could be used for quality control of hawthorn lipid-lowering soft capsules