CAJ | 학술논문

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品粒,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 mmi.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4.5×10~4,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.
자제료자외-가견분광광도계적미주전영고효분리부건,개소료X사선연사법재전영미주제비중적응용이급미주전영여자외-가견분광광도법적재선련용.사용수열법합성균균석영미미품립,채용X사선연사법표정화공제산물적정상,병용소묘전자현미경관찰산물형모.장합성적석영미미정립균균전충재2 mmi.d.석영관중,제성전영미주.통과미주전영여자외-가견분광광도법재선련용,대비연생적색안산、분병안산화락안산진행료분리검측.검출한분별위0.037,0.20화0.20 μmol·L~(-1),색안산적분리효솔위매미4.5×10~4,전영미주적양품용량체도35 μL.실험결과표명,전충석영미미정립적미주전영가억제대주경전영열효응,증대양품용량,제고검측령민도.미주전영여상규자외-가견분광광도법련용가간편지대혼합물진행재선분리화측정,진일보탁관료자외-가견분광광도계재광보중첩조분흔량분석중적응용.
In the present paper,a laboratory-made high-performance electropboresis microcolumn unit was prepared for UV-Vis spectrophotometer.X-ray diffraction was used in the preparation of electrophoretic microcolurnns.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.The quartz microncrystals were packed into a 2-mm i.d.fused-silica tube to prepare the electrophoretic mierocolumn.With 1.5 mmol·L~(-1) disodium phosphate buffer solution (pH 11.5) containing 25% (ψ) methanol and 10% (ψ) acetonitrile,tryptophan,phenylalanine and tyrosine were on-line separated on line and detected by microcolumn electrophoresis coupled with UV-Vis spectrophotometry without derivatization.The limits of detection were 0.037,0.20 and 0.20 μmol·L 1,respectively.The separation efficiency of tryptophan was 4.5×10~4 plates/m.The sample capacity of the electrophoretic microcolumn achieved 35 μL.It was found that the electrophoretic microcolumn packed with quartz microncrystals was able to limit Joule heat,increase sample capacity and enhance detection sensitivity.The laboratory-made electrophoretic microcolumn could be a high-performance separation unit for conventional UV-Vis spectrophotometer.The on-line coupling of microcolumn electrophoresis and UV-Vis spectrophotometry could separate and determine samples with complicated matrices,reduce zone broadening and enhance separation efficiency,so expand the analytical function of speetrophotometer in the trace analysis of mixed components with overlapped spectra.