CAJ | 학술논문

以甲基丙烯酸缩水甘油酯(GMA)为单体,二乙烯基苯(DVB)为交联剂,以环己醇和正十二醇为致孔剂,过氧化苯甲酰(BPO)为引发剂,直接以50 mm×4.6 mm色谱柱为模具,通过原位聚合制备聚(GMA-DVB)型整体柱.以GMA和DVB的体积比、环己醇和十二醇的体积比以及BPO占聚合物的质量分数为三因素,以分离苯和乙苯等小分子物质时的半峰宽分离度(R_(1/2))为考察指标,进行三因素三水平的正交试验,通过测定整体柱的比表面积、孔径和孔容分布对其进行表征.结果表明,制备整体柱的最优配方为 V(GMA): V(DVB)∶ V(环己醇)∶ V(正十二醇)=0.825∶0.825∶1.32∶2.03,BPO的质量分数为0.7% .应用所制备的整体柱分离苯和乙苯等小分子物质,理论塔板数达到 37 000 塔板/m,R_(1/2)值达到7.14,完全达到基线分离,分离时间小于10 min.该方法制备整体柱的重复性好,柱效较高,基本满足商品化要求.
이갑기병희산축수감유지(GMA)위단체,이을희기분(DVB)위교련제,이배기순화정십이순위치공제,과양화분갑선(BPO)위인발제,직접이50 mm×4.6 mm색보주위모구,통과원위취합제비취(GMA-DVB)형정체주.이GMA화DVB적체적비、배기순화십이순적체적비이급BPO점취합물적질량분수위삼인소,이분리분화을분등소분자물질시적반봉관분리도(R_(1/2))위고찰지표,진행삼인소삼수평적정교시험,통과측정정체주적비표면적、공경화공용분포대기진행표정.결과표명,제비정체주적최우배방위 V(GMA): V(DVB)∶ V(배기순)∶ V(정십이순)=0.825∶0.825∶1.32∶2.03,BPO적질량분수위0.7% .응용소제비적정체주분리분화을분등소분자물질,이론탑판수체도 37 000 탑판/m,R_(1/2)치체도7.14,완전체도기선분리,분리시간소우10 min.해방법제비정체주적중복성호,주효교고,기본만족상품화요구.
A monolithic column of macro porous poly(glycidyl methacrylate-divinylbenzene) (poly(GMA-DVB)) has been prepared by free radical polymerization within the confines of a chromatographic stainless steel tube (50 mm×4.6 mm).For the best separation and low back pressure,orthogonal experiments were carried out with V(cyclohexanol)∶ V(dodecanol),V(GMA)∶ V(DVB) and BPO dosage as the three main factors.The characteristic feature of the column,including specific surface area,pore volume as well as pore diameter distribution,was studied by scanning electron microscopy (SEM),mercury intrusion porosimetry analysis and BET analysis.The obtained optimum preparation conditions were that the volume ratio of GMA,DVB,cyclohexanol and dodecanol was 0.825∶0.825∶1.32∶2.03 and the BPO dosage was 0.7%(mass percentage),then it was heated at 70 ℃ for 24 h.Using this monolithic column,benzene and ethylbenzene and a drug of oxiracetam can be well separated on a high performance liquid chromatographic (HPLC) system equipped with a ultraviolet (UV) detector at 254 nm.A solution of acetonitrile-water (50∶50,v/v) for the separation of benzene and ethylbenzene,and acetonitrile-water (80∶20,v/v) for the separation of oxiracetam were used as mobile phases at a flow rate of 1 mL/min.The theoretical plate number was 37 000 plates/m and the resolution of peak width at half height (R_(1/2)) was 7.14.The separation time was less than 10 min.The monolithic column prepared by this method is reproducible and has high column efficiency.It is an economical method to prepare monolithic column,which can be applied to separate small molecules.