HPLC法测定参苓健体粉中去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯Ⅲ和白术内酯Ⅰ

Determination of dehydrotumulosic acid,dehydropachymic acid,pachymic acid,atracylenolide Ⅲ,and atracylenolide Ⅰ in Shenling Jianti Powder by HPLC

目的：建立梯度洗脱联合波长切换高效液相色谱（HPLC）法对参苓健体粉中去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯Ⅲ和白术内酯Ⅰ同时进行测定。方法采用Venusil MP C18色谱柱（250 mmx4.6 mm，5μm）；流动相：乙腈–0.05%磷酸溶液，梯度洗脱；检测波长：210 nm（0-19 min，检测去氢土莫酸、去氢茯苓酸和茯苓酸）、220 nm（19-35 min，检测白术内酯Ⅲ和白术内酯Ⅰ）；体积流量：0.8 mL/min；柱温：30℃；进样量为10μL。结果去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯III、白术内酯I质量浓度分别在4.62-92.40μg/mL（r＝0.9997）、3.80-76.00μg/mL（r＝0.9999）、5.76-115.20μg/mL（r＝0.9999）、3.95-79.00μg/mL（r＝0.9998）、5.05-101.00μg/mL（r＝0.9996）与峰面积关系良好；回收率分别为99.24%、97.75%、98.66%、98.49%、99.10%，RSD值分别为1.23%、1.79%、1.66%、0.80%、1.25%。结论建立的方法操作简便、结果可靠，可用于参苓健体粉的质量控制。

Objective To develop an HPLC-wavelength switching method for simultaneous determination of dehydrotumulosic acid, dehydropachymic acid, pachymic acid, atracylenolide III, and atracylenolide I in Shenling Jianti Powder. Method The Venusil MP C18 column （250 mm ＆#215; 4.6 mm, 5μm） was adopted;the mobile phase was acetonitrile-0.05%phosphoric acid solution with gradient elution, with a flow rate of 0.8 mL/min. The column temperature was set at 30 ℃, and injection volume was 10 μL. Results Dehydrotumulosic acid, dehydropachymic acid, pachymic acid,atracylenolide III and atracylenolide I had good linearity in the ranges of 4.62—92.40 μg/mL （r=0.999 7）, 3.80—76.00 μg/mL （r=0.999 9）, 5.76—115.20 μg/mL （r=0.999 9）, 3.95—79.00 μg/mL （r=0.999 8）, and 5.05—101.00 μg/mL （r=0.999 6）, respectively. The average recoveries were 99.24%, 97.75%, 98.66%, 98.49%, and 99.10% with RSD of 1.23%, 1.79%, 1.66%, 0.80%, and 1.25%, respectively. Conclusion The method is rapid and with high accuracy which can be applied to the quality control of Shenling Jianti Powder.