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目的:建立HPLC法测定利胆排石片中柚皮苷、橙皮苷、新橙皮苷、槲皮苷和黄芩苷的含量。方法:采用ZORBAX C18(250mm×4.6mm,5μm)色谱柱,以甲醇(A)-4%乙酸水溶液(B)两相溶剂梯度洗脱[0～20min,20%A→40%A;20～30min,40%A;30～45min,40%A→52%A],流速0.8mL·min-1,检测波长280nm。结果:在选定条件下,柚皮苷、橙皮苷、新橙皮苷、槲皮苷和黄芩苷达到良好分离,分别在1.91～490μg·mL-1(r=0.9996),2.02～216μg·mL-1(r=0.9996),1.14～292μg·mL-1(r=0.9997),2.73～700μg·mL-1(r=0.9998),3.91～1000μg·mL-1(r=0.9998)范围内,浓度与峰面积呈良好线性关系,平均回收率分别为99.2%,98.5%,95.5%,95.1%,98.1%。结论:本方法简便可靠,适合于利胆排石片的质量控制。
Objective: To establish HPLC method for the determination of naringin, hesperidin, neohesperidin, quercitrin and baicalin in Lidan Paishi tablets. Methods: ZORBAX C18 (250mm×4.6mm, 5μm) column was used to elute with methanol (A)-4% acetic acid aqueous solution (B) two-phase solvent gradient [0～20min, 20%A→40%A; 20～ 30 min, 40% A; 30-45 min, 40% A→52% A], flow rate 0.8 mL·min-1, detection wavelength 280 nm. RESULTS: Under the selected conditions, naringin, hesperidin, neohesperidin, quercitrin and baicalin were well separated, and they were 1.91-490 μg·mL-1 (r=0.9996) and 2.02-216 μg respectively. In the range of mL-1 (r=0.9996), 1.14 to 292 μg·mL-1 (r=0.9997), 2.73 to 700 μg·mL-1 (r=0.9998), 3.91 to 1000 μg·mL-1 (r=0.9998), The concentration and peak area showed a good linear relationship. The average recoveries were 99.2%, 98.5%, 95.5%, 95.1%, and 98.1%, respectively. Conclusion: This method is simple and reliable, and it is suitable for the quality control of Lidan row stone tablets.