取五灵脂药材(1.0 g)与海沙3.0 g混匀,置于加速溶剂萃取(ASE)仪中,加入萃取溶剂［乙醇-水(75+25)］静态萃取循环3次,每次10 min,萃取温度为100 ℃,压力为15 MPa。萃取液蒸缩至3 mL,加C2H5OH-H2O(75+25)至5.0 mL,过滤后供液相色谱分析。在色谱分离中,以Diamosil ODS C18色谱柱为固定相,用(A)甲醇和(B)乙酸(0.5+99.5)溶液以不同比例的混合液作为流动相进行梯度淋洗。在波长360 nm处进行检测。药材中的芦丁、山奈酚和穗花杉双黄酮的质量浓度与相应的峰面积之间呈线性关系,3种组分的检出限(3S/N)在0.3~0.6 mg·kg-1之间。在3个浓度水平条件下用标准加入法进行回收试验,测得回收率在80.0%~95.0%之间,测定值的相对标准偏差(n=5)在3.2%~9.6%之间。

Three components (i.e. rutin, kaempferol and amentoflavone) in faeces trogopterori sample (10 g) was extracted with mixture of C2H5OH-H2O (75+25) thrice for 10 min each in an accelerated solvent extractor under temperature of 100 ℃ and pressure of 15 MPa. The extracts were combined and evaporated to ca. 3 mL;after cooling, its volume was made up to 5.0 mL with the C2H5OH-H2O (75+25) mixture, and the solution was separated on the chromatographic column of Diamosil ODS C18 and eluted gradiently with mixtures of (A) methanol and (B) 0.5% (φ) acetic acid solution with various mixing ratios. UV detection at 360 nm was used in the determination. Linear relationships between values of peak area and mass concentrations of the 3 components were found in definite ranges, with detection limits (3S/N) ranged from 0.3 to 0.6 mg·kg-1. Recovery was tested by standard addition at 3 concentration levels, giving results of recovery in the range of 80.0% to 95.0%, with values of RSD′s (n=5) ranged from 3.2% to 9.6%.