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目的:优化马钱苷、丹皮酚和毛蕊花糖苷的HPLC方法,检测山药硫熏前后的六味地黄丸中3种成分含量的差异,研究硫熏对复方的影响。方法:采用Thermo Hypersil BDS C18色谱柱（4.6 mm×250 mm,5μm）。马钱苷,流动相乙腈-0.1%磷酸梯度洗脱,检测波长236 nm;丹皮酚,流动相乙腈-0.1%磷酸（50∶50）,检测波长274 nm;毛蕊花糖苷,流动相乙腈-0.1%乙酸梯度洗脱,检测波长334 nm。柱温30℃,流速1 m L·min-1,进样量10μL。结果:随SO2量的增加,六味地黄丸中丹皮酚、马钱苷和毛蕊花糖苷均有明显的下降趋势,亚硫酸钠组的3种成分含量最低,分别为0.022 6,0.691 2,0.036 2 mg·g-1。结论:该研究优化的HPLC方法准确灵敏、重复性好,适合用于六味地黄丸的含量测定。结果证实硫熏山药对六味地黄丸会有不利影响,其根源在于SO2残留。 Objective: To optimize HPLC methods of loganin,paeonol and verbascoside,we detected the content of three components in Liuwei Dihuang Wan that prepared by sulfur-fumigated Dioscoreae Rhizoma,in order to reveal the effect of sulfur-fumigation on Traditional Chinese Medicine formulae. Method: The column was a Thermo Hypersil BDS C18( 4. 6 mm × 250 mm,5 μm). Loganin was gradiently eluted by acetonitrile-0. 1%phosphoric acid with water system as mobile phase,and 236 nm as the detection wavelength. Paeonol was isocraticly eluted by acetonitrile-0. 1% phosphoric acid with water( 50 ∶ 50),and 274 nm as the wavelength.Verbascoside was gradiently eluted by acetonitrile-0. 1% phosphoric acid with water system as mobile phase,and236 nm as the wavelength. The column temperature was 30 ℃,the flow rate was 1 m L·min-1,the injection volume was 10 μL. Result: With the increase of SO2 amount,loganin,paeonol and verbascoside derived from Liuwei Dihuang Wan were obviously decreased. In thesodium sulfite group,the content of the three components was the lowest,which to 0. 022 6,0. 691 2 and 0. 036 2 mg·g-1. Conclusion: The optimized HPLC methods had good accuracy,sensitivity and repeatability,which was suitable for determining in Liuwei Dihuang Wan. The results indicated that sulfur-fumigated Dioscoreae Rhizoma would have an adverse effect on Liuwei Dihuang Wan;the possible reason came from SO2 residue.