| The wastewater produced from Gansu Kushui rose essential oil production enterprise(Hereinafter referred to as "rose wastewater")has high concentration of organic matter,high chroma,great difficulty in treatment,high cost of treatment,direct discharge or substandard discharge,which not only causes waste of resources,but also seriously affects the environment.Such wastewater contains available components such as polyphenols.Through the purification,separation,antioxidant screening,preparation method and identification of pure substances in rose wastewater,not only can the polyphenols in wastewater be recovered,but also the polyphenols can be used as non-toxic and healthy food additives.In line with the national circular economy industrial policy;Moreover,in the process of recycling,the color of waste water becomes lighter,the content of organic matter is greatly reduced,the difficulty of wastewater treatment is reduced,and the environmental pollution is improved.The main research contents and experimental results of this paper are as follows:1.The purification conditions of polyphenols in rose wastewater were studied.On the one hand,the standard curve was made,and the total polyphenol content in wastewater was determined,the content of which was 5.428 mg/m L.On the other hand,the polyphenols in wastewater were enriched and purified by D101 resin,and the purification conditions were determined by static and dynamic adsorption and resolution experiment.The results were as follows: Dry resin 2g,sample p H 3,sample concentration 2.714 mg/m L,adsorption flow rate 1 m L/min,sample volume 65 m L;elution flow rate 1 m L/min,Ethanol concentration 80%,Ethanol volume 18 m L.Under the purified conditions,the adsorption rate and the resolution rate reached77.83% and 82.76%,and the recovery rate was 67.31%.After the purification of the wastewater,Polyphenol purity was increased from 2.208% to 29.48%,and increased by 14.54 times.2.The total antioxidant activity of polyphenol from wastewater purified solution was studied.The scavenging ability of DPPH·?ABTS·+?·OH and so on were determined.The half inhibitory concentration(IC50 value)was respectively 0.832mg/L,0.371 mg/L,0.371 mg/L,19.28 mg/L,which was 7 times,17 times,1.5 timesas much as Gallic acid,and was 30 times,23 times,3 times as much as ascorbic acid.3.A method for the separation of polyphenols from rose oil distillation wastewater by UPLC was established and the methodology was investigated.the 15 polyphenols had a good linear relationship in the range of 1~400 ?g/m L(R2>0.9963);the repeatability,the relative standard deviation of intra-day and inter-day precision were less than 2%;the recovery rate was 86.41%~ 103.87%,and the relative standard deviation was 0.7~2.1%;the detection limit(S/N?3)was 0.2 mg/kg.Moreover,the chromatogram before and after the reaction of polyphenols from wastewater with hydroxyl radical was compared by using the established method,then the antioxidant activity of each substance was obtained.The results showed that 12 components were screened out,among them,peak 19 and 22 had the strongest and weakest scavenging ability to hydroxyl radical,which were respectively 59.37% and 35.77%;while the other 10 components had different scavenging rates,but all of them were about 50%,The numerical difference is not obvious.In a word,all of these 12 components have obvious antioxidant activity.4.A preparation chromatography method was established to prepare polyphenols with high content and good antioxidant activity from wastewater.Combined with UPLC chromatographic method,it was found that the B peak was completely overlapped with peak 1,and analyzed qualitatively by Q-TOF-MS/MS,It was proved that the sample B was a Gallic acid. |
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