余甘子加工沉淀固废物中活性成分鉴定与提取工艺优化

Identification of Active Components from Precipitated Solid Waste of Phyllanthus emblica and Optimization of the Extraction Process

目的:研究余甘子鲜汁沉淀物的化学组成与资源化物质鞣花酸的提取纯化工艺。方法:收集余甘子鲜汁沉淀物,采用能谱仪、傅里叶变换红外光谱仪和超高效液相色谱与串联四极杆飞行时间质谱联用技术(UPLC-Q-TOF-MS)分析余甘子鲜汁沉淀物的化学成分;以鞣花酸含量为指标,分别采用醇提法、酶提法、碱溶酸沉法对鞣花酸进行提取纯化,且通过单因素实验优化筛选提取工艺。结果:红外分析表明,余甘子鲜汁沉淀物具有C、O元素,苯环、酚羟基等基本结构;UPLC-Q-TOF-MS结果表明,沉淀物的主要成分为鞣花酸、邻苯二甲酸二丁酯等,且鞣花酸占比最高,为39.91%;提取工艺优化结果显示,碱溶酸沉法为较优工艺,进一步优化后得到最佳工艺参数为料液比1∶40、NaOH浓度2%、超声提取时间20 min,该条件下得到的提取物中鞣花酸含量为47.38%,纯度为94.22%。扫描电镜观察表明,鞣花酸提取物粉末中有大量柱状结晶,推测为鞣花酸分子平面聚合形成。结论:余甘子鲜汁沉淀物中鞣花酸天然丰度高,可作为鞣花酸天然来源途径之一。所得到的鞣花酸提取纯化工艺步骤简单、可操作性强、成本较低、含量及纯度较高,适宜用于余甘子鲜汁固废物中鞣花酸的富集。

Objective:To study the chemical composition of fresh juice precipitate from Phyllanthus emblica and the extraction and purification process of resource material ellagic acid.Methods:The precipitate of fresh juice of P.emblica was collected,and the chemical composition of its fresh juice precipitate was analyzed by energy dispersive spectrometer(EDS),Fourier transform infrared spectroscopy(FT-IR),and ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS).Taking the content of ellagic acid as the index,the extraction and purification of ellagic acid were carried out by alcohol extraction,enzyme extraction,and alkali-solution-acid sedimentation method,and the extraction process was optimized by the single-factor experiment.Results:Infrared analysis showed that the fresh juice precipitate of P.emblica mainly contained C and O elements,benzene ring,phenolic hydroxyl group,and other basic structures.The results of UPLC-Q-TOF-MS showed that the main components were ellagic acid and dibutyl phthalate,and the proportion of ellagic acid was the highest(39.91%).The optimized extraction process results showed that the alkali-solution-acid sedimentation method was the superior technology,and the optimal parameters were 1∶40 of solid-liquid ratio,2%of NaOH concentration,and 20 min of ultrasonic extraction time.Under these conditions,the content of ellagic acid in the extract was 47.38%,and the purity was 94.22%.The results of scanning electron microscopy showed that there were a large number of columnar crystals in the extract powder of ellagic acid,which were presumably formed by the planar polymerization of ellagic acid molecules.Conclusion:The natural abundance of ellagic acid in the fresh juice precipitate of P.emblica is high,which can be used as one of the natural sources of ellagic acid.The extraction and purification process of ellagic acid obtained in this study is simple and feasible with low cost,high content,and high purity,which is suitable for the enrichment of ellagic acid in the fresh juice precipitate of P.emblica.