Yu Chang-Zhu, He You-Zhao, Han Fang, Fu Guo-Ni
Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026, China.
J Chromatogr A. 2007 Nov 9;1171(1-2):133-9. doi: 10.1016/j.chroma.2007.09.046. Epub 2007 Sep 22.
A post-column reactor with coaxial-gap mode is developed for laser-induced fluorescence detection (LIF) in capillary electrophoresis (CE). The reactor can be assembled simply and conveniently, in which a thin polyimide sleeve of 10-mm length obtained from the capillary coating is used to align separation and reaction capillary with a 20 microm gap. Naphthalene-2,3-dicarboxaldehyde and 2-mercaptoethanol are used as derivatization reagents and delivered into the reaction capillary through the annulus between the separation capillary and polyimide sleeve and the gap of two capillaries by gravity. A reaction distance from the gap to detection point is 5mm. For the post-column reactor of CE-LIF, several configuration parameters are optimized, including liquid level difference between the derivatization solution and outlet buffer, annular dimension between the outer diameter of etched separation capillary and the inner diameter of polyimide sleeve, and reaction distance, etc. The detection limits in the range from 8.0x10(-8) to 1.0x10(-6) mol/L and linear calibration range more than two orders of magnitude are obtained for amino acids. The separation efficiency ranges from 1.35x10(5) to 1.67x10(5) theoretical plates.
开发了一种具有同轴间隙模式的柱后反应器,用于毛细管电泳(CE)中的激光诱导荧光检测(LIF)。该反应器组装简单方便,使用从毛细管涂层获得的10毫米长的薄聚酰亚胺套管,以20微米的间隙对齐分离毛细管和反应毛细管。萘-2,3-二甲醛和2-巯基乙醇用作衍生试剂,通过分离毛细管和聚酰亚胺套管之间的环形空间以及两根毛细管的间隙,靠重力输送到反应毛细管中。从间隙到检测点的反应距离为5毫米。对于CE-LIF柱后反应器,优化了几个配置参数,包括衍生化溶液与出口缓冲液之间的液位差、蚀刻分离毛细管外径与聚酰亚胺套管内径之间的环形尺寸以及反应距离等。氨基酸的检测限在8.0×10⁻⁸至1.0×10⁻⁶mol/L范围内,线性校准范围超过两个数量级。分离效率为1.35×10⁵至1.67×10⁵理论塔板数。