聚二乙烯基苯微球制备及其在小分子和多肽反相色谱分离中应用

以二乙烯基苯为原料，采用微孔膜乳化法制备了尺寸均一的乳液，在75℃下悬浮聚合24 h，制得均一的聚二乙烯基苯微球，对其表面形态、粒径及其分布进行了表征，并考察了微球的色谱分离性能. 结果表明，微球呈多孔球体结构，粒径约为25 mm，平均孔径为14 nm，比表面积达520 m2/g，且机械强度好(可耐40~50 MPa高压). 利用该微球装填的半制备级高效液相色谱柱(300 mm×10 mm I.D.)分别分离酚类混合物和多肽混合物，分离度均大于1.5，最大理论塔板数分别达13000和21000 m-1，批次间重现性良好.

Preparation of Uniform Polydivinylbenzene Microspheres and Their Application in Reversed-phase Chromatographic Separation of Small Molecular Compounds and Peptides

Taking divinylbenzene as monomer, polydivinylbenzene (PDVB) microspheres with particle size 25 mm were prepared by membrane emulsification and suspension polymerization at 75℃. Their morphology and size distribution of pores were investigated, their application in reversed-phase chromatographic separation of small molecular compounds and peptides examined. The prepared PDVB microspheres had uniform particle size (span value=0.91), mean pore size of 14 nm, specific surface area of 520 m2/g, and high mechanical intensity (keeping stable under 40~50 MPa pressure). The PDVB microspheres were packed into semi-preparative columns (300 mm×10 mm I.D.) and tested by separating phenol derivatives and peptides mixture on high performance liquid chromatography. The resolution of both systems was higher than 1.5, and theoretical plate number reached 13000 and 21000 m-1, respectively. PDVB microspheres showed perfect batch to batch reproducibility on separation. They would be a promising reversed-phase stationary phase for preparative and process purification of peptides.