知母药材和饮片含量测定修订研究

目的: 建立全面反映和控制知母药材和饮片质量状况的含量测定方法。 方法: HPLC-UV法测定知母中芒果苷含量,采用Kromasil C₁₈柱(4.6 mm×250 mm,5 μm),流动相为乙腈-0.2%醋酸水溶液(15∶ 85),流速1 mL·min^-1,检测波长258 nm; HPLC-ELSD法测定知母皂苷BII含量,采用C₈柱(4.6 mm×250 mm,5 μm),流动相为乙腈-水(25∶ 75),流速0.8 mL·min^-1,蒸发光散射检测器蒸发温度为105 ℃,雾化气体流速为2.7 L·min^-1。 结果: 芒果苷在8.4~420 μg·mL^-1范围内浓度与峰面积呈良好的线性关系(r²=0.9997),平均回收率(n＝6)为103.2%,RSD为0.7%。知母皂苷BII在101.2~1012 μg·mL^-1范围内其浓度的常用对数与峰面积的常用对数呈良好的线性关系(r²=0.9993),平均回收率(n＝6)为104.0%,RSD为2.2% 。不同操作者测定两种成分,含量测定结果偏差RSD均小于3.0%。 结论: 本文所建立的含量测定方法具有较高的专属性,准确、简便、耐用性好,是控制知母药材和饮片质量的较理想方法。

Objective: To establish an assay method for quality control of Anemarrhenae Rhizoma. Methods: HPLC-UV method is adopted to determine the content of mangiferin.Kromasil C₁₈ column(4.6 mm×250 mm,5 μm) was used as stationary phase.Mobile phase was acetonitrile-0.2% acetic acid(15∶ 85)with the flow rate of 1 mL·min^-1 ,detect wavelength was 258 nm.HPLC-ELSD method is adopted to determine the content of timosaponin BII.C₈ column(4.6 mm×250 mm,5 μm) was used as stationary phase.Mobile phase was acetonitrile-water(25∶ 75),with the flow rate of 0.8 mL·min^-1.The temperature of evaporation was 105 ℃ and the gas flow rate was 2.7 L·min^-1. Results: There was good linearity in the range of 8.4-420 μg·mL^-1 for mangiferin(r²=0.9997),the average recovery was 103.2% with RSD of 0.7%(n＝6).Timosaponin BII has good linearity in the range of 101.2-1012 μg·mL^-1(r²=0.9993),the average recovery was 104.0% with RSD of 2.2%(n＝6).The differences of the results by different operators in these two compounds determination are both within 3.0%. Conclusion :The assay method is rapid and accurate,having good endurance.It is suitable for quality control of Anemarrhenae Rhizoma.