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目的:建立高效液相色谱法测定垂盆草配方颗粒中槲皮素、山奈素及异鼠李素含量的方法。方法:流动相为甲醇:0.4%磷酸溶液(45:55),色谱柱为Diamonsil C_(18)(200 mm×4.6 mm,5μm),检测波长为360 nm,柱温为30℃,流速为1.0 ml·min~(-1)。结果:三种黄酮类成分分离度好,不受杂质干扰,线性范围:槲皮素在2.982～29.820μg·ml~(-1),r=0.999 7,山奈素在0.966～9.660μg·ml~(-1),r=0.999 8,异鼠李素在0.982～9.820μg·ml~(-1),r=0.999 4;平均回收率:槲皮素99.26%,RSD=0.66%(n=6),山奈素99.21%,RSD=1.24%(n=6),异鼠李素99.44%,RSD=0.40%(n=6)。结论:该测定方法操作简便,快捷,可靠性高,重复性好,可作为垂盆草配方颗粒的质量控制方法之一。
Objective: To establish a method for the determination of quercetin, kaempferol and isorhamnetin in sibiricum granules by high performance liquid chromatography. METHODS: The mobile phase consisted of methanol: 0.4% phosphoric acid solution (45:55), the column was Diamonsil C18 (200 mm × 4.6 mm, 5 μm), the detection wavelength was 360 nm, the column temperature was 30 ℃ and the flow rate was 1.0 ml · min ~ (-1). Results: The separation of the three flavonoids was good without interference from impurities. The linear ranges of quercetin were 2.982 ~ 29.820μg · ml -1, r = 0.999 7, and kaempferol were between 0.966 ~ 9.660μg · ml ~ (-1), r = 0.999 8, isorhamnetin at 0.982-9.820μg · ml -1, r = 0.999 4; average recovery was 99.26% of quercetin, RSD was 0.66% (n = 6 ), Kaempferol 99.21%, RSD = 1.24% (n = 6), isorhamnetin 99.44%, RSD = 0.40% (n = 6). Conclusion: The method is simple, rapid, reliable, reproducible and can be used as one of the quality control methods for sodagraph particles.