微柱电泳与紫外-可见分光光度法的在线联用

自制了紫外-可见分光光度计的微柱电泳高效分离附件, 介绍了X射线衍射法在电泳微柱制备中的应用以及微柱电泳与紫外-可见分光光度法的在线联用。使用水热法合成均匀石英微米晶粒，采用X射线衍射法表征和控制产物的晶相，并用扫描电子显微镜观察产物形貌。将合成的石英微米晶粒均匀填充在2 mm i.d.石英管中，制成电泳微柱。通过微柱电泳与紫外-可见分光光度法在线联用，对非衍生的色氨酸、苯丙氨酸和酪氨酸进行了分离检测。检出限分别为0.037, 0.20和0.20 μmol·L-1，色氨酸的分离效率为每米4.5×104，电泳微柱的样品容量达到35 μL。实验结果表明，填充石英微米晶粒的微柱电泳可抑制大柱径电泳热效应，增大样品容量，提高检测灵敏度。微柱电泳与常规紫外-可见分光光度法联用可简便地对混合物进行在线分离和测定，进一步拓宽了紫外-可见分光光度计在光谱重叠组分痕量分析中的应用。

On-Line Coupling of Microcolumn Electrophoresis and UV-Vis Spectrophotometry

In the present paper,a laboratory-made high-performance electrophoresis microcolumn unit was prepared for UV-Vis spectrophotometer.X-ray diffraction was used in the preparation of electrophoretic microcolumns.And an analytical technique of microcolumn electrophoresis coupled with UV-Vis spectrophotometry was introduced.Uniform quartz microncrystals were prepared by hydrothermal synthesis.Their crystalline phase and morphology were identified by X-ray diffraction and scanning electron microscope,respectively...