目的建立同时测定白术药材中白术内酯Ⅰ、Ⅱ、Ⅲ和苍术酮含量的HPLC法。方法采用Dikma Diamonsil C8色谱柱(150 mm×4.6 mm,5μm),以乙腈-水为流动相,梯度洗脱,检测波长为220和275 nm,流速为1.0 m L·min-1,柱温为30℃。结果白术内酯Ⅰ、Ⅱ、Ⅲ和苍术酮质量浓度分别在1.304~3.912 mg·L-1、1.126~3.378 mg·L-1、1.740~5.220 mg·L-1和47.60~142.8 mg·L-1内线性关系良好。平均加样回收率分别为96.9%、95.4%、96.7%和95.8%,RSD分别为1.2%、1.7%、1.6%和1.3%(n=9)。结论该方法简便、准确、重复性好,可用于白术药材的质量控制。
Objective To establish an HPLC method for simultaneous determination of the contents of atractylenolide I,II,III and atractylon in Atractylodes macrocephala Koidz.. Methods Separation was carried out on a Dikma Diamonsil C8column( 150 mm × 4. 6 mm,5 μm) with a gradient mobile phase composed of acetonotrile and water at a flowrate of 1. 0 m L·min- 1. The detection wavelength was set at 220 and 275 nm and the column temperature was 30 ℃. Results The linear ranges of calibration curve for atractylenolide I,II,III and atractylon were 1. 304- 3. 912 mg·L- 1,1. 126- 3. 378 mg·L- 1,1. 740- 5. 220mg·L- 1and 47. 60- 142. 8 mg·L- 1( r≥0. 999 2),respectively. The average recoveries of atractylenolide I,II,III and atractylon were 96. 9%,95. 4%,96. 7% and 95. 8% and the relative standard deviations( RSDs) were 1. 2%,1. 7%,1. 6% and 1. 3%( n = 9),respectively. Conclusions This method is simple,accurate and reproducible for the quality control of Atractylodes macrocephala Koidz..