大果紫檀心材色素纯化及成分研究

Purification and composition of heartwood pigment of Pterocarpus macrocarpus

【目的】研究大果紫檀心材色素的纯化工艺及成分,为其心材形成机理提供理论基础。【方法】以大果紫檀心材为原料,使用7种溶剂抽提大果紫檀心材色素,测定波长并建立心材色素质量浓度的标准曲线。选用10种大孔树脂纯化心材色素,分别测定吸附率、吸附量、解吸率和解吸量,确定吸附效果最佳的树脂。在DA-201树脂的动态吸附过程中,以色素质量浓度为指标探究不同因素的影响大小,确定最佳吸附条件。使用超高效液相色谱串联四极杆–静电场轨道阱高分辨质谱仪联用技术(UPLC-Q-EXCTIVE-MS)对纯化后的心材色素分离与鉴定。【结果】选用乙醇作为提取溶剂,提取液的色差值为55.15。将486 nm作为测定波长,建立了标准曲线。大孔树脂DA-201的吸附–解吸值最佳,其吸附量和吸附率分别是10.07 g/L和80.19%,解吸量和解吸率分别是7.06 g/L和70.07%。在DA-201大孔树脂的静态吸附过程中,最佳条件为pH值4和洗脱剂乙醇浓度100%。在动态吸附过程中,最佳吸附条件分别为吸附流速2.0 mL/min,上样液质量浓度2 g/L;最佳解吸条件分别为洗脱流速1 mL/min,洗脱剂用量100 mL。对纯化后的心材色素分析,从中分离鉴定出10种黄酮类和醇类化合物,分别为荭草苷、牡荆素、金雀异黄素、白藜芦醇、白杨素、黄豆黄素、异甘草素、诺卡酮、芒柄花黄素和酮洛芬。【结论】用DA-201型大孔吸附树脂纯化大果紫檀心材色素工艺稳定,获得了最佳吸附和解吸条件,同时确定了心材色素成分。

[Objective]In order to provide scientific basis for forming mechanism of Pterocarpus macrocarpus heartwood,we investigated the purification process of heartwood pigment and component identification.[Method]The pigment of Pterocarpus macrocarpus heartwood was extracted by 7 solvents.The wavelength was measured to established a standard curves of the heartwood pigment concentration.In the purification process of the heartwood pigment,absorption efficiency,absorption concentration,desorption efficiency and desorption concentration of 10 kinds of macroporous resins were measured to determine the resin with the best absorption effect.In the process of dynamic absorption and desorption,the mass concentration of pigment was used as an indicator to explore the influence of different factors on DA-201 macroporous resin,and then determine the best absorption process.UPLC-Q-EXCTIVE-MS was used to separate and identify the components of purified pigment.[Result]Ethanol was selected as the extraction solvent,and the chromatic aberration of solutions was 55.15.The 486 nm was used as the measurement wavelength to establish a standard curve.The optimum absorption conditions of DA-201 were as follows:static absorption concentration was 10.07 g/L,absorption rate was 80.19%.The optimum desorption conditions of DA-201 were as follows:static desorption concentration was 7.06 g/L,desorption rate was 70.07%.In the static absorption process of DA-201 macroporous resin,the optimum conditions were:pH value was 4,eluent ethanol concentration was 100%.In the dynamic absorption process of DA-201 macroporous resin,the optimal absorption conditions for pigment were:the absorption flow rate was 2.0 mL/min,the mass concentration of the sample solution was 2 g/L.The optimum conditions of desorption effect were:the elution flow rate was 1 mL/min and the eluent volume was 100 mL.UPLC-Q-EXCTIVEMS was used to separate and identify 10 flavonoids and alcohol compounds from the purified pigment,which were orientin,vitexin,genistein,resveratrol,chrysin,glycitein,isoliquiritin,nocarone,formononetin,ketoprofen.[Conclusion]DA-201 macroporous resin can purify the pigment of Pterocarpus macrocarpus heartwood effectively,and the components of the pigment are determined simultaneously.