反相高效液相色谱法同时测定参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量

Simultaneous Determination of Atractylenolide Ⅱ and Ⅲ in Shenling Baizhu Granule by RP-HPLC

目的建立一种同时测定白术内酯Ⅱ和白术内酯Ⅲ的高效液相色谱检测方法，并分析中成药参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量。方法样品采用液-液萃取，以乙腈-水（50∶50）为流动相，流速1.0 ml·min^-1，采用SH IMADZU ODS柱（150 mm×4.6 mm；5μm）色谱柱分离；检测波长220 nm。结果标准曲线线性范围为0.5-50.0μg·ml^-1，线性关系良好（r〉0.99），定量限为0.5μg/ml，回收率98%以上，方法的稳定性、重复性和精密度均较好（RSD〈3%）。结论该法操作简便、快速、灵敏、准确，已经成功地用于中成药参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量测定。

Objective To develop an HPLC - UV method for the simultaneous determination of atractylenolide Ⅱ and Ⅲ and to detect the content of atractylenolide Ⅱ and Ⅲ in Chinese medicinal preparation. Methods After a simple liquid - liquid extraction, atractylenolide Ⅱ and Ⅲ were separated on SHIMADZU C18 column（4.6 mm× 150 mm, 5 μm） and detected by UV spectrometry. The detection wavelength was set at 220 nm. The mobile phase consisted of acetonitrile - water （50： 50） at a flow rate of 1.0 ml · min ^-1. The content of atractylenolide Ⅱ and Ⅲ in Chinese medicinal preparation（ Shenling Baizhu Granule） was simultaneously determined by the method above after simple liquid - liquid extraction. Results The linear calibration curves were obtained in the concentration range of O. 5 - 50.0 μg·ml^-1 （ r 〉 0.99）. The lower limit of quantification was 0.5μg·ml^-1. The recoveries were more than 98.0% , and the stability, repeatability and precision of the method were all better in all cases（ RSD 〈 3% ）. Conclusion The RP - HPLC method is specific, simple, sensitive and accurate. And this method was successfuly applied to simultaneously quantitate atraetylenolide Ⅱ and Ⅲ in Chinese medicinal preparation （Shenling Baizhu Granule）.