Isolation And Purification Of Syringin And The Oleuropein From Syringa Reticulata Var.mandshurica Sprig

In this paper,medicinal plants Syringa reticulata var.mandshurica sprig as raw material,ionic liquid-lithium salt based microwave pretreatment followed by ultrasonic-assisted extraction of syringin and oleuropein from Syringa reticulata var.mandshurica sprig by a dual response surface methodology.The response surface method of mircrowave pretreatment stage and ultrasonic assisted extraction phase extraction process was optimized.Macroporous resin enrich and purify syringin and oleuropein of ionic liquid-lithium salt extraction.The main contents are as follows:Set up HPLC method which was for determining the content of syringin and oleuropein.Chromatographic separation was carried out by a Kromasil-C18(5μm3 4.6 mm×250 mm)reversed-phase column,the mobile phase is methanol-water-phosphoric acid(40:60:0.5,v:v:v).syringin and oleuropein was separation at the wavelength of 232 nm.The flow rate was 1 mL/min,the injection volume was 10 μL and the column temperature was maintained at 25℃,retention time was 40 min.Ionic liquid-lithium salt based microwave pretreatment followed by ultrasonic-assisted extraction of syringin and oleuropein,taking response surface method to optimize for its extraction conditions.The different types and amount of ionic liquids and lithium salt,microwave pretreatment temperature,time,ultrasonic power and time,solid-liquid ratio to impact for yield of syringin and oleuropein.The optimum extraction conditions:the optimum extraction solvent[C4mim]Br and LiCl,the amount of[C4mim]Br is 11.76 mmol,and LiCl 77 mg,microwave pretreatment temperature is 95℃,1.5 min,ultrasonic power 228 W,solid-liquid ratio 1:20,extraction time is 13 min,and oleuropein syringin total yield are 6.21 mg/g.Macroporous resin enrich and purify syringin and oleuropein of ionic liquid-lithium salt extraction were studied.By comparing 11 kinds of macroporous resin:HPD600,DM130,ADS-7,HPD100B,ADS-17,HPD417,HPD-400A,HPD-300L,D101,HPD80,HPD750 to the ability of adsorption and desorption for syringin and oleuropein.We believe that HPD100B is the ideal resin for the enrichment and purification of syringin and oleuropein.The optimum adsorption parameters of HPD100B:the optimal sample volume is 200 mL,the sample flow rate 2 BV/h,the adsorption temperature of 25℃.Syringin adsorption capacity was 4.03 mg/g,oleuropein was 70.32 mg/g.The optimal desorption parameters of macroporous resin HPD100B:First,with 20%ethanol eluted syringin and collected 6 BV,and then with 40%ethanol eluted oleuropein and collected 10 BV.Syringin and oleuropein can be eluted from the resin,respectively.Elution flowrate 1 BV/h.The purity of syringin is 1.2%,and the oleuropein is 10%.Ionic liquid-lithium salt based microwave pretreatment,ultrasonic assisted completely break the plant cell wall,so that the target product dissolve out from the cell.And by using macroporous resin enrich and separate target products to improve the purity.This method is rapid,effective,low cost.And this method had not been reported.