以枝形大分子聚酰胺-胺(PAMAM)为键合固定相的开管毛细管电色谱柱的制备及评价

用3-氨丙基三乙氧基硅烷(KH550)作偶联剂, 在毛细管内壁上逐步合成树枝形大分子聚酰胺-胺(PAMAM), 制得了1, 2和3代PAMAM键合的开管毛细管电色谱柱, 并对其性能进行了研究. 结果表明， 随着大分子代数的增加, 毛细管电渗流(EOF)逐步下降. 利用制得的1， 2和3代PAMAM修饰的开管毛细管电色谱柱对丙氨酸和脯氨酸的分离进行对比, 结果显示, 随着大分子PAMAM代数的增加, 分离度逐步增大, 丙氨酸和脯氨酸可在3代树枝状大分子PAMAM修饰的开管毛细管电色谱柱上达到基线分离. 采用非衍生化法和3代PAMAM修饰的开管毛细管电色谱柱成功地分析了精氨酸、 丙氨酸、 脯氨酸、 甲硫氨酸和组氨酸. 结果表明， 键合毛细管柱具有良好的重现性和稳定性.

Preparation and Evaluation of Open-tubular Capillary Electrochromatography Column with the Poly(amidoamine)(PAMAM) Dendrimers as Bonded Stationary Phase

The objective of our study is to explore the potential of poly(amidoamine)(PAMAM) dendrimers as a bonded stationary phase in open tubular capillary electrochromatography(CEC).1G,2G and 3G poly(amidoamine)(PAMAM) dendrimers were bonded to the interior wall of silica capillaries through a(3-aminopropyltriethoxysilane) linker step by step.The obtained columns were characterized by CEC process.The results show that the electroosmotic flow(EOF) gradually reduced with increasing PAMAM generation.The performances of the column were evaluated by the separation of alanine and praline.The results indicate that the resolution of alanine(Ala) and proline(Pro) was gradually improved with increasing the amount of PAMAM generation.By open-tubular capillary electrochromatography column modified with the 3rd generation PAMAM,the baseline separation of the alanine and proline can be obtained.Five underivatized amino acids,arginine(Arg),alanine(Ala),proline(Pro),histidine(His) and methionine(Met),were successfully separated by OCEC modified with 3G PAMAM and by using UV detection at 200 nm.The reproducibility and stability of the column were satisfactory.