【作者】 刘军；

【导师】 方群；

【作者基本信息】 浙江大学 ， 分析化学， 2005， 硕士

【摘要】 微流控系统在分析化学中变得越来越重要。微系统中不同的检测方法对被分析物的定性和定量是必不可少的。然而由于微加工芯片的结构特点,在毛细管电泳和液相色谱中广泛应用的紫外-可见吸收光度检测方法,在微流控芯片系统中的应用受到很大限制。虽然有文献报道解决上述问题,但通常分析系统的结构相当复杂。本论文中提出了基于缺口型试样管阵列试样引入系统的微型化紫外检测毛细管电泳系统,并将其用来快速分离复方新诺明片中的磺胺甲噁唑(SMZ)和甲氧苄氨嘧啶(TMP)。此外,还进行了玻璃芯片鞘流型紫外检测毛细管电泳系统的初步研究。 在第一章中,介绍了在微流控芯片系统中紫外-可见吸收光度检测技术的进展和应用,对文献中不同的紫外-可见吸收光度检测模式进行了详细综述,讨论了在微流控芯片系统实现吸收光度检测存在的困难。 在第二章中,详细综述了H-通道微流控毛细管电泳系统的发展现状,包括通过与其联用的流动注射和顺序注射等连续进样系统,以及不同的检测系统,如激光诱导荧光检测,发光二极管诱导荧光液芯波导检测,电化学检测,化学发光检和紫外检测。 在第三章中,实现了基于缺口型试样管阵列的微流控试样引入系统与紫外检测-毛细管电泳系统的联用,建立可实现自动化、高通量、连续试样引入的微型化毛细管电泳系统。试样引入系统由底部加工有缺口的试样管阵列构成,阵列固定一维平移台上。实验时,通过平移试样管阵列,使毛细管和电极依次经缺口进入装有试样或缓冲液的试样管内,完成电动进样和电泳分离操作。该系统被用来快速分离复方新诺明片中的磺胺甲噁唑(SMZ)和甲氧苄氨嘧啶(TMP),以考察系统分析性能。分析通量达到72样/h,试样间携出量为1.4%,对SMZ的分离塔板高度11μm。采用紫外检测对SMZ和TMP检测限(3σ)分别为9.8mg/L和12.2mg/L。 在第四章中,初步进行了玻璃芯片毛细管电泳鞘流型紫外检测系统的研究,初步结果证明了技术路线的可行性。更多还原

【Abstract】 Microfluidic systems have become more and more important in the field of analytical chemistry. Various detection methods on these microsystems are essential for the identification and quantification of chemical species that are being analyzed. UV/Vis absorbance detection has widely applied in CE and HPLC systems. However, its application in microfabricated chips has been limited owing to the short optical path-length in planar chip structures. Efforts have been made to overcome such limitations, with some success, but resulting in rather sophisticated structures. In this dissertation, a miniaturized capillary electrophoresis system with slotted micro-vial array based sample introduction system and UV detection was developed and applied in fast separation of sulphamethoxazole (SMZ) and trimethoprim (TMP) in sulphatrim tablets. In addition to the previous work, a UV absorbance detection system with sheath flow configuration for glass CE chip was also developed for the first time.In the first chapter, the development of UV/Vis absorbance detection system on microfluidic chips and its applications were reviewed. The difficulties of realizing a robust UV/Vis absorbance detection system are discussed.In the second chapter, the development of microfluidic H-channel system for rapid CE separations was reviewed. Applications of the system, coupling to flow-injection and/or sequential-injection sample introduction, for the determination of FITC- labeled amino acids by laser-induced fluorescence or LED-induced fluorescence with liquid core waveguide detection , trace metals by chemi-luminescence, carbohydrates by amperometry, and drugs by UV absorbance are exemplified to illustrate the performance and versatility of the microfluidic system.In the third chapter, a high throughput sample introduction system based on slotted micro-vial array was coupled to a miniaturized capillary electrophoresis(CE) system with short capillary and UV detection to achieve automated and continuous sample introduction and separation in CE system. The sample introduction system is composed of an array of horizontally positioned micro-sample vials with slits fabricated on the bottom of each vial. Sample introduction was performed by linearlymoving the array of vials, allowing the capillary and electrode to sequentially enter the solutions in the vials through the slits achieving sample introduction and separation operation. The present system was applied in fast separation of sulphamethoxazole (SMZ) and trimethoprim (TMP) in sulphatrim tablets, achieving a high throughput of 72 h"1 and a low carryover of 1.4%. Separation efficiency of 11 urn plate height for SMZ was obtained. The detection limits (3a) for SMZ and TMP were 9.8 mg /L and 12.2 mg /L, respectively.In the fourth chapter, a sheath flow configuration flow-cell coupled to two optic fibers was designed to achieve the UV detection on glass CE chip-based system.更多还原