采用液相色谱-静电场轨道阱高分辨质谱法(LC-Orbitrap HRMS)对阿尔泰金雀花中的黄酮类化合物进行鉴定分析。称取过筛后的样品粉末20.0 g,按料液比1 g∶50 mL加入60%(体积分数)乙醇溶液,于60℃超声提取50 min,经抽滤、减压浓缩、干燥后得粗提物;采用AB-8型大孔吸附树脂对粗提物进行纯化,将粗提液按2.8 BV的柱床体积、2.5 mL·min^-1的流量进样,再用70%(体积分数)乙醇溶液以2.0 BV的柱床体积,3.0 mL·min^-1的流量进行洗脱,收集洗出液,减压浓缩、干燥后得到金雀花精提物;称取金雀花精提物5 mg,用甲醇溶解并定容至10 mL,过滤,得到供试品溶液。以Waters C₁₈色谱柱为固定相,以不同体积比的乙腈-0.2%(体积分数)甲酸溶液为流动相进行梯度洗脱。质谱分析采用电喷雾离子源负离子模式,扫描范围质荷比(m/z)为100~1 100。结果显示,根据一级质谱图确定的化合物精确相对分子质量和二级质谱碎片离子信息,参考国内外相关文献,从阿尔泰金雀花中鉴定出21种黄酮类化合物,并对化合物的裂解途径进行分析,为探讨阿尔泰金雀花的药效物质基础提供了理论依据。

Flavonoid compounds in Altai Caragana sinica were identified and analyzed by liquid chromatography-orbitrap high resolution mass spectrometry (LC-Orbitrap HRMS). The sifted powder sample (20.0 g) was taken and extracted ultrasonically in 60% (φ) ethanol solution (at the ratio of material mass to liquid volume on 1 g∶50 mL) at 60 ℃ for 50 min. After suction filtration, vacuum concentration and drying, the crude extract obtained was injected at a column bed volume of 2.8 BV, flow rate of 2.5 mL·min^-1, and eluted with 70% (φ) ethanol solution at a column bed volume of 2.0 BV, flow rate of 3.0 mL·min^-1 for purification by AB-8 macroporous adsorption resin, then the eluate was collected for vacuum concentration and drying. 5 mg of the refined extract obtained was taken and its volume was made up to 10 mL with methanol, and the test solution was obtained after filtering. Waters C₁₈ column was used as stationary phase, and a mixture of acetonitrile and 0.2% (φ) formic acid solution at different volume ratios was used as mobile phase for gradient elution. Electrospray ion source with negative mode was adopted in MS analysis, and the scanning range was m/z 100-1 100. As shown by the results, according to the precise relative molecular weight of compounds determined by the primary MS, the fragment ions information from the secondary MS and referring to relevant literatures at home and abroad, and 21 flavonoid compounds were identified in Altai Caragana sinica and the fragment pathways of compounds were analyzed, which provided theory basis for elucidating the pharmacodynamic material foundation of Altai Caragana sinica.