HPLC-ELSD法测定苍耳子及其制剂中羧基苍术苷和苍术苷含量

Determination of Carboxyatractyloside and Atractyloside in Xanthii Fructus and its Preparation with High Performance Liquid Chromatography Evaporative Light-Scattering Detector

目的：建立苍耳子及其制剂（辛芩片和辛芩颗粒）中毒性成分羧基苍术苷和苍术苷的高效液相色谱-蒸发光散射检测器（HPLC-ELSD）定量测定方法。方法：采用Kromasil 100-5C18色谱柱（4.6 mm×250 mm,5μm）,以乙腈（A）-10 mmol/L乙酸铵溶液（B）为流动相,梯度洗脱（0-30 min,12%A→20%A;30-31 min,20%A→12%A;31-35 min,12%A）,柱温35℃,体积流量1.0 m L/min,蒸发光散射检测器检测（漂移管温度95℃,N2载气流速1.6 L/min）。结果：羧基苍术苷在0.681-4.086μg线性关系良好,线性回归方程为Y=1.4973X＋3.9461（r=0.9996）,平均回收率96.4%（n=6,RSD=1.2%）;苍术苷在0.731-4.383μg线性关系良好,线性回归方程为Y=1.4619X＋4.0630（r=0.9991）,平均回收率97.7%（n=6,RSD=0.9%）。结论：HPLC-ELSD法定量测定羧基苍术苷和苍术苷方法简便,重复性良好,可用于苍耳子及其制剂的质量控制。

Objective：To develop a high Performance liquid chromatography evaporative light-scattering detec- tor（HPLC-ELSD） for determining contents of two poisonous eomponents,carboxyatraetyloside and atraetyloside in Cangerzi（Xanthii Fructus） and its preparation（Xinqin tablets and Xinqin granules）. Method：A Kromasil 100-5C18 column（4.6 mm×250 mm,5 μm） with the mobile phase consisting of acetonitrile（A）-10 mmol/L and ammonium acetate solution （B）, in gradient elution manner （0- 30 min, 12%A→20%A ; 30- 31 min, 20%A→12% A;31--35 min,12%A）. The column temperature was 35 ℃ and the flow rate was 1.0mL/min. The drift tube temperature of ELSD was set at 95 ℃ with the N2 flow rate at 1.6 L/min. Result：Carboxyatractyloside and atraetyloside exhibit good linearity within the ranges from 0.681 to 4.086 p,g and from 0.731 to 4.383 μg,respectively. The regression equations were Y=1.4973X＋3.9461 （r=0.9996） and Y=1.4619X＋4.0630（r=0.9991） ; the average recovery rate （n=6） was 96.4% （RSD=1.2%） and 97.7% （RSD=0.9%）, respectively. Conclusion ：The established HPLC-ELSD method was simple and repeatable,and it could be applied to the quality control of Xanthii Fructus and its preparation.