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目的建立蒲黄中香蒲新苷和异鼠李素-3-O-新橙皮苷的含量测定方法。方法采用单因素考察方法建立供试品溶液制备方法;采用高效液相色谱法(HPLC)法测定香蒲新苷和异鼠李素-3-O-新橙皮苷的含量,色谱条件为Waters SunFire~(TM)C_(18)(4.6 mm×250 mm,5μm)色谱柱,乙腈-0.05%磷酸溶液梯度洗脱,流速1.0 m L/min,检测波长254 nm,柱温20℃。结果蒲黄药材采用80倍量的甲醇回流提取1.5 h,制备供试品溶液;香蒲新苷在0.245 2~1.471 0μg范围内线性关系良好,r=0.999 9,平均加样回收率为98.47%,相对标准偏差(RSD)=2.05%(n=6);异鼠李素-3-O-新橙皮苷在0.191 2~1.147 4μg范围内线性关系良好,r=0.999 7,平均加样回收率为100.56%,RSD=2.56%(n=6)。结论所建立的含量测定方法简便准确,重现性好,为蒲黄药材质量控制和评价奠定基础。
Objective To establish a method for the determination of cattail glycosides and isorhamnetin-3-O-neohesperidin in Puhuang. Methods The single-factor method was used to establish the method for the preparation of the test solution. The content of the taxol and isorhamnetin-3-O-neohesperidin was determined by high performance liquid chromatography (HPLC). The chromatographic conditions were Waters SunFire ~ (TM) C18 (4.6 mm × 250 mm, 5 μm) column with gradient elution of acetonitrile-0.05% phosphoric acid solution at a flow rate of 1.0 mL / min with a detection wavelength of 254 nm and a column temperature of 20 ℃. Results Puhuang herbs were extracted with 80 times of methanol by refluxing for 1.5 h to prepare the test solution. The calibration curve was linear in the range of 0.245 2 ~ 1.471 0 μg with r = 0.999 9 and the average recovery was 98.47% The relative standard deviation (RSD) was 2.05% (n = 6). The calibration curve of isorhamnetin-3-O-neohesperidin was linear in the range of 0.191 2 ~ 1.147 4 μg with r = 0.999 7. 100.56%, RSD = 2.56% (n = 6). Conclusion The established method for the determination of content of Puhuang herbs is simple, accurate and reproducible, which lays the foundation for the quality control and evaluation of Puhuang herbs.