3种苍术的特征图谱及苍术素醇、苍术素和白术内酯Ⅱ含量测定研究

目的:建立关苍术与茅苍术、北苍术的特征图谱,并对3种苍术中苍术素醇、苍术素和白术内酯Ⅱ含量进行测定。方法:采用HPLC法, Promosil C₁₈色谱柱(4.6 mm×250 mm, 5μm),以乙腈-磷酸水为流动相,梯度洗脱,流速1.0 mL·min^-1,检测波长270 nm,柱温25℃。结果:建立了3种苍术特征图谱,确认了苍术素醇、苍术素和白术内酯Ⅱ 3个特征峰。苍术素醇、苍术素和白术内酯Ⅱ质量浓度分别在0.0004~0.0119 mg·mL^-1(r=0.9997)、0.0011~0.2175 mg·mL^-1(r=0.9999)、0.0028~0.0522 mg·mL^-1(r=0.9997)范围内呈良好线性关系;平均加样回收率(n=9)分别为98.0%、99.2%和98.7%。不同产地苍术中苍术素醇、苍术素和白术内酯Ⅱ含量范围分别为0.06~0.41、0.21~10.96和0.19~2.67 mg·g^-1。结论:关苍术与茅苍术、北苍术特征图谱差异较大,苍术素醇、苍术素和白术内酯Ⅱ含量相差也较大。HPLC法可快速鉴别关苍术与茅苍术、北苍术,特征图谱与含量测定方法结合,操作简单,结果准确,重现性好,为全面评价苍术质量提供可靠的分析方法。

Objective:To develop specific chromatograms and an HPLC method for analyses of atractylodinol, atractylodin and atractylenolide Ⅱ in the rhizomes of Atractylodes japonica, A. lancea and A. chinensis. Methods:The Promosil C 18(4.6 mm×250 mm, 5μm)column was adopted to separate the sample at the column temperature of 25℃. The mobile phase consisted of acetonitrile-phosphoric acid aqueous with a gradient elution at a flow rate of 1.0 mL·min^-1. The detection wavelength was set at 270 nm. Results:The specific chromatograms of the rhizomes of A. japonica, A. lancea and A. chinensis were developed, which identified peaks of atractylodinol, atractylodin and atractylenolide Ⅱ. The calibration curves were linear in the ranges of 0.0004-0.0119 mg·mL^-1 for atractylodinol(r=0.9997), 0.0011~0.2175 mg·mL^-1 for atractylodin(r=0.9999)and 0.0028-0.0522 mg·mL^-1 for atractylenolide Ⅱ(r=0.9997). The average recovery rates were 98.0%, 99.2% and 98.7%,respectively. The contents of atractylodinol, atractyldtylodin and atractylenolideⅡwere 0.06-0.41 mg·g^-1,0.21-10.96 mg·g^-1 and 0.19-2.67 mg·g^-1 in Rhizoma Atractylodis from different production regions, respectively. Conclusion:There is a considerable difference between the rhizomes of A. japonica and both the rhizomes of A. lancea and A. chinensis in specific chromatograms. The contents of atractylodinol, atractylodin and atractylenolide Ⅱalso have a considerable difference. HPLC method can be used to quickly identify the rhizomes of A. japonica, A. lancea and A. chinensis. The method of specific chromatograms combined with compounds determination is simple and reproducible, and thus can be used for the quality control of Rhizoma Atractylodis.