Application Research And Chiral Separation Of Cinchona Alkaloidsby Capillary Electrophoresis Based On The Chiral Ionic Liquids

Objective:This paper studied the cinchona alkaloid extraction and separated methods, discussed the separation mechanism of the enantioseparation of four cinchona alkaloids(quinine, quinidine,cinchonine,cinchonidine)using the mixture of HP-β-CD and [TBA][L-ASP] as selectors in capillary electrophoresis. A kind of economic, fast, efficient, green environmental capillary electrophoresis method was set up eventually and successfully used for quantification of underivatized cinchona alkaloid in Cinchona tree bark, Compound quinine injection, Watsonstonic wa ter. Method:(1) In the first place, taking advantage of organic reagent methanol as the extraction solvent, and using ultrasonic extraction method for four cinchona alkaloid study. The effect of the related parameters consist of ultrasonic frequency, ultrasonic time, temperature, the volume of the ammomia solutionby the method of ultrasonic extraction were investigated. A good extraction C inchona tree bark was achieved in the end.(2) In pressure injector, uncoate capillary column(75μm×57cm), combination with HP-β-CD and the [TBA][L-ASP] as selectors, andammonium acetatebackground electrolytecondition, capillary electrophoresis was used toseparation and detection the four epimer Cinchona alkaloids. The related separation parameters, such as HP-β-CD and [TBA][L-ASP] concentrations,buffer concentrations, p H, separation voltage and temperature were investigated.Ultimately, a good capillary electrophoresis separation and detection condition was achieved. 40 m M HP-β-CD, p H5.0, 14 m M [TBA][L-ASP], 25 m M ammonium acetate, the wavelength was 235 nm, the applied voltage of 15 k V and column temperature 25℃. Results:(1) 20 m L methanol and 2m L ammomia were added in 1.5g medical material power. Then ultrasound 30 min in 70 Hz and 40℃ before the crude drugs soaked 1h. Under optimum condition the best extraction rate was achieved by using C E to test.(2) Under the electrophoresis optimum conditions, the linearity of four cinchona alkaloids(quinine, quinidine, cinchonine, cinchonidine) was achieved within concentration ranges from 1 to 500 μg/m L and the correlation coefficients R2 were 0.9975,0.9994,0.9990,0.9986 respectively. The intra RSD<4.0% and the inter RSD<4.1%; The recovery of actual sampleswas ranged from 95.9% to 102.9%, and the analytes were separated in less than 7min. Conclusions:In order to improve thesensitivity and reproducib ility of the analytein capillary electrophoresis, a variety of chiral reagentcould been choose. Combined use of HP-β-CD and [TBA][L-ASP] as chiral selective reagents at same time for chiral separation of alkaloids by capillary electrophoresiscould make the method more simple, economy and effective.