高效液相色谱-蒸发光散射检测法同时测定四君子丸中的5种有效成分

Simultaneous determination of five effective components in Sijunzi bolus using high performance liquid chromatography-evaporation light scattering detection

建立了同时测定四君子丸中党参炔苷、茯苓酸、甘草酸、苍术内酯Ⅲ和白术内酯Ⅰ含量的高效液相色谱法。色谱条件为:HIQSILC18V色谱柱(250mm×4.6mm,5μm),以0.5%冰乙酸-甲醇体系为流动相进行梯度洗脱,流速为1.0mL/min,采用蒸发光散射检测器检测,进样量为10μL,柱温为25℃,漂移管温度为55℃,喷雾器加热级别为60%,载气为氮气,压力0.2MPa。在上述条件下,党参炔苷、茯苓酸、甘草酸、苍术内酯Ⅲ和白术内酯Ⅰ的质量浓度分别在0.076～1.21,0.048～0.76,0.153～2.45,0.045～0.72和0.098～1.56g/L时,质量浓度的对数值与色谱峰面积的对数值之间的线性关系良好;平均回收率在97.13%～100.25%之间,相对标准偏差在1.23%～2.44%之间。该方法简便、快速、准确,可用于四君子丸的质量控制。

A high performance liquid chromatographic （HPLC） method was developed for the simultaneous determination of lobetyolin, pachymic acid, glycyrrhizic acid, atractylenoide Ⅲ and atractylenolideⅠ in Sijunzi bolus. The separation was performed on an HIQ SIL C18 V column （250 mm×4.6 mm, 5 μm） with 0.5% acetic acid-methanol as the mobile phase of gradient elution at a flow rate of 1.0 mL/min. The detection was performed with an evaporation light scattering detector （ELSD） and the sample volume was 10 μL. The temperature of drift tube and heating grade of nebulizer was respectively set at 55 ℃ and 60% at 0.2 MPa of pressure. Nitrogen gas was used as carrier gas. Under the optimized conditions, there were good linear relationships between the logarithm values of mass concentration and the peak areas of lobetyolin, pachymic acid, glycyrrhizic acid, atractylenoide Ⅲ and atractylenolide Ⅰ in the ranges of 0.076-1.21, 0.048-0.76, 0.153-2.45, 0.045-0.72 and 0.098-1.56 g/L, respectively. The recoveries of the five components were between 97.13% and 100.25%, the relative standard deviations （RSDs） were between 1.23% and 2.44%. This method is simple, rapid, accurate and suitable for the quality control of Sijunzi bolus.