Preparation Of Polymer Chromatography Packing By Post-crosslinking Method For The Purification Of Scutellarin

In this paper, the poly (styrene-divinylbenzene) microspheres with the size of15μm was prepared by the seed swelling method using polystyrene microspheres with the size of3μm.The particle size and dispersion were investigated to study the mass ratio of the swelling agent,the catalyst and the dispersant on the synthesis of poly(styrene-divinylbenzene) microspheres.The optimal synthesis conditions were as follows:the mass ratio of the swelling agent and seeds was3,the mass ratio of the benzoyl peroxide(BPO) and the monomers was0.015,the mass ratio of the polyvinyl alcohol and reaction system was0.013.Under the above conditions,the low degree of crosslinking and highly crosslinked PS-DVB microspheres were synthesized using the isooctanol and toluene as the porogen.then the polymer chromatography packing of high specific surface area was prepared by Friedel-Crafts post-crosslinking reaction of polystyrene microspheres of low degree of crosslinking using a,a’-dichloro-p-xylene as crosslinking agent and by post-crosslinking reaction of pendant vinyl groups of polystyrene microspheres of highly degree of crosslinking.The polymer chromatography packing with the larger surface area was applied to the purification of scutellarin.The column(4.6mmx250mm) packed by the above packing was applied to the HPLC separation of scutellarin,resolution,selectivity and retention time was investigated to study the proportion of mobile phase, the mobile phase flow rate,column temperature and sample concentration on the separation process of scutellarin.Under the follow conditions:the proportion of mobile phase (acetonitrile/0.4%glacial acetic acid)27:73(v/v),the flow rate1.OmL/min,column temperature30℃,sample concentration300μg/mL,the resolution was2.20,the two components were separated completely.then column(36.6mmx207mm) packed by the above packing was applied to the medium pressure preparative liquid chromatography(MPLC) purification of scutellarin,Purity and recovery of scutellarin was investigated to study the proportion of mobile phase, the mobile phase flow rate and sample concentration on the purification process of scutellarin.At last we obtained scutellarin products with purity of97.6%and recovery of86.2%.providing an effective new approach for the industrial production of scutellarin.