Study On The Extraction And Purification Process Of Echinacoside And Acteoside In Cistanche Deserticola Y.C.Ma

Echinacoside and acteoside are the main chemical constituents of Cistanche deserticola Y.C.Ma in the Orobanchaceae genus Cistanche.A rapid,efficient and simple method for the analysis and detection of echinacoside and acteoside in C.deserticola was established by high performance liquid chromatography(HPLC).Ionic liquid surfactants(ILs)with ultrasonic-assisted methods was used to optimize extraction process of C.deserticola.Macroporous adsorption resin was used to separate phenylethanol glycosides,magnetic molecular imprinting technology was used to enrich the echinacoside and acteoside in the resin desorption solution,and pyrolysis was used to prepare C.deserticola residue biochar.Finally,the adsorption performance of C.deserticola residue biochar was evaluated and characterized.1.Establish an analytical method for simultaneous determination of echinacoside and acteoside in C.deserticola by HPLC.Analysis conditions are as follows:HIQ sil C18W Column(4.6 mm × 250 mm,5μm)were used for separating echinacoside and acteoside.Acetonitrile-0.4%Formic acid solution(A)-acetonitrile(B)as the mobile phases and the elution process was 0-6 min,90%(A);6-16 min,90-80%(A);16-20 min,80-75%(A);20-25 min,75-80%(A);25-30 min,80-90%(A)at a wavelength of 333 nm with 1.0 mL/min of flow rate.The results show that the method is sensitive,accurate and stable,and it provides a method for the quantification of echinacoside and acteoside in C.deserticola.2.Synthesize ILs[C10mim]Br,[C12mim]Br and[C14mim]Br through the quaternization method using an ultrasonic-microwave synergistic device;through the aqueous phase method,[C10mim][BF4],[C12mim][BF4]and[C14mim][BF4]were prepared by the metathesis reaction in aqueous solution.The effect of ILs with different carbon chain lengths,anions and cations on the extraction of echinacoside and acteoside in C.deserticola was investigated.And[C12mim][BF4]aqueous system for the extraction of echinacoside and acteoside was optimized by single factor experiment and response surface method.The conventional alcohol extraction,water ultrasonic extraction,ionic liquid surfactant extraction and the traditional extraction methods of C.deserticola were compared.The extraction yields of echinacoside and acteoside from C.deserticola with ILs was the highest,reaching 7.47 mg/g and 3.56 mg/g,respectively.In addition,through the resin enrichment of echinacoside and acteoside in the[C12min][BF4]aqueous system,the recycling ability of the recovered[C12mim][BF4]aqueous system was investigated.Four cycles of extraction have examined the recycling capacity of the recovered[C12mim][BF4]aqueous system.The relative regeneration rate of the recovered[C12mim][BF4]aqueous system for the extraction of the target compound can reach more than 90%.3.The macroporous adsorption resins were used to enrich and purify the crude extract of C.deserticola.Six kinds of macroporous adsorption resins were screened through static adsorption and desorption,and the best resins were used for thermodynamic experiments and dynamic analysis experiments.The recovery rates of echinacoside and acteoside were 89.67%and 88.92%respectively.4.The dual-template magnetic MCM-41 mesoporous molecular sieve molecularly imprinted polymer(Fe3O4@MCM-41-MIPs)was synthesized using echinacoside and acteoside as template molecules,Fe3O4 MCM-41 mesoporous molecular sieve as a magnetic material,4-vinylpyridine(4-VP)as a functional monomer and azobisisobutyronitrile(AIBN)as a porogen.To study the structural morphology of the polymer,infrared spectroscopy and transmission electron microscopy were used for characterization analysis.The adsorption performance of the polymer was investigated through adsorption kinetics test and isothermal adsorption test.The results showed that the Fe3O4@MCM-41-MIPs was successfully prepared and has good selective adsorption to phenyl ethanol glycosides.After separation,the content of phenylethanol glycosides was determined to reach 91.85%,and the purity of echinacoside and acteoside were 33.5%and 27.0%respectively.5.The biochar preparation of C.deserticola residue was carried out,and the factors affecting the preparation of biochar were optimized.The adsorption capacity of C.deserticola residue biochar for phenol and methylene blue was investigated.Multiple cycles of desorption were carried out to investigate the reutilization ability of the C.deserticola residue biochar,and to characterize the biochar before and after adsorption.The results showed that the phenol adsorption capacity of C.deserticola residue biochar under optimal conditions was 29.75 mg/g,and it could be cyclically adsorbed three times.