目的 基于麦冬经不同程度硫熏后，相关检测指标的变化情况，优化麦冬硫熏的适宜工艺。方法 运用苯酚-硫酸法测定麦冬多糖的量；运用HPLC-ELSD法测定麦冬皂苷D和D'的量，流动相为乙腈-水（50∶50），漂移管温度40 ℃，氮气体积流量2.0 L/min；运用HPLC-UV法进行麦冬正丁醇部位指纹图谱研究，流动相为乙腈-0.1%磷酸水梯度洗脱，检测波长297 nm，同法测定甲基麦冬二氢高异黄酮A和B的量。以硫熏麦冬的总多糖、麦冬皂苷D和D'、甲基麦冬二氢高异黄酮A和B的质量分数及指纹图谱得分为综合考察指标，以硫磺用量和硫熏时间为考察因素，运用星点设计-效应面法优化麦冬硫熏工艺。结果 在实验设计范围内，随着硫磺用量和硫熏时间的增加，多糖的量先增加后降低，麦冬皂苷D和D'的量轻微增加后降低，甲基麦冬二氢高异黄酮A和B的量逐步降低。最终确定麦冬硫熏工艺为硫磺用量120~200 g/m³，硫熏时间0.6~1.5 h，多元2项式方程为Y=0.574＋0.054 3 X₁－0.008 13 X₂－0.518 X₁²＋0.131 X₂²＋0.153 X₁X₂，R-Sq=0.971。工艺验证结果表明偏差绝对值小于3%。结论 本研究明确麦冬硫熏后相关化学成分变化情况，建立适宜麦冬的硫熏工艺。

Objective To optimize the suitable technology of Ophiopogon japonicus (OJ) fumigation based on the changes of relative indexes after the different levels of sulfur fuming. Methods The phenol-sulfuric acid method was used to determine the content of polysaccharide. HPLC-ELSD method was used to determine the contents of Ophiopogon saponins D (OPD) and D' (OPD') with the mobile phase of acetonitrile-water (50:50), drift tube temperature at 40℃, and nitrogen volumetric flow of 2.0 L/min. The fingerprints of OJ were determined by HPLC-UV method, the mobile phase was eluted with acetonitrile-0.1% phosphoric acid gradient, and the detection wavelength was 297 nm. The contents of ethylophiopogonanones A (MA) and B (MB) were determined using the same method. Using the contents of total polysaccharides of OJ, OPD and OPD', MA and MB, and the contents of other components in the fingerprints as control indexes, and the dosage of sulfur and the time of sulfur fumigation as factors, the central composite design-response surface methodology (CCD-RSM) was used to optimize sulfur fumigation process. Results In the experimental design range, the content of polysaccharides increased first and then decreased with the increase of sulfur dosage and sulfur fumigation time, and the contents of OPD and OPD' increased slightly and then decreased. The contents of MA and MB were slightly reduced. The sulfur fuming process was determined as follows:sulfur dosage was 120-200 g/m³, sulfur fuming time was 0.6-1.5 h, binomial equation:Y=0.574+0.054 3 X₁-0.008 13 X₂-0.518 X₁²+0.131X₂²+0.153 X₁X₂ (R-Sq=0.971). Process validation:the absolute value of deviation was less than 3%. Conclusion In this study, the changes of chemical composition of OJ were studied, and the sulfur smelting process suitable for OJ was established.

山西省中医药研究院院级课题（201508）