【作者】 孙永华；

【导师】 章竹君；

【作者基本信息】 陕西师范大学 ， 分析化学， 2006， 硕士

【摘要】 本论文由综述和研究报告两部分组成。综述部分简单概述了液相色谱化学发光检测的历史、原理、仪器结构、用于液相色谱柱后检测的主要化学发光体系以及该技术面临的挑战和机遇。研究报告部分包括：液相色谱化学发光法测定盐酸青藤碱、液相色谱化学发光法测定鞣花酸、液相色谱化学发光法测定柚皮甙和液相色谱化学发光法测定穿琥宁。 随着人们对化学发光技术研究的不断进步，对化学发光的了解也不断深入。化学发光分析法不需要外部光源，消除了杂散光及因光源发光不稳定而导致波动的缺点，从而降低了噪声，提高了信噪比，再加上灵敏的光电检测技术，使该法具有灵敏度高、线性范围宽、设备简单、易于实现自动化等优点；但该方法也有选择性差的缺点，从而限制了它的应用。将它和色谱等分离手段结合，成为人们自然的设想，即利用色谱将被分析物分离后用化学发光法进行高灵敏度的检测，这样就可以克服化学发光法选择性差的缺点。另外，和常用的传统液相色谱检测器如紫外检测器比较，化学发光检测法在许多情况下有着更高的灵敏度；因而，可以实现对这些物质的高灵敏度检测。自1974年Hartkopf等首次报道了液相色谱化学发光检测法以来，该技术发展迅速，已成为一种分析和测量复杂基质中痕量和超痕量组分的有力工具，被广泛研究和应用于冶金、化工、医药、环境、生物医学科学、临床化学等领域。 1 高效液相色谱化学发光法测定盐酸青藤碱 基于盐酸青藤碱对高锰酸钾-硫代硫酸钠的化学发光的增敏作用，建立了反相高效液相色谱分离柱后化学发光检测盐酸青藤碱的新方法，并成功用于血样和尿样中盐酸青藤碱的测定。该方法的线性范围为：5.0×10^-7—5.0×10^-5g／mL，检出限为：8×10^-8g／mL（S／N=3），对盐酸青藤碱溶液连续11次测定的相对标准偏差为：2.8％。 2 高效液相色谱化学发光法测定鞣花酸 Co（Ⅱ）和鞣花酸的配合物对luminol-H₂O₂在碱性条件下的发光反应的催化作用比Co（Ⅱ）更强；基于此，建立了液相色谱化学发光测定鞣花酸的新方法。将该方法用于测定石榴皮中鞣花酸的含量，并和液相色谱紫外检测进行了比较，结果令人满意。方法的线性范围为：5.0×10^-8g／mL—5.0×10^-6g／mL检出限为：2×10^-8g／mL（S／N=3）。更多还原

【Abstract】 This thesis includes two sections—review and research report. In the review section, informations about high performance liquid chromatography-chemiluminescence detection （HPLC-CL） such as history, principles, HPLC-CL equipment and the main chemiluminescence reaction systems used in HPLC-CL was summarized. In the next research report section, four applied reports about HPLC-CL for determination of sinomenine hydrochloride（SIN）, Ellagic acid（EA）,Naringin and Potassium Sodium Dehydroandroan drographolide Succinate （DAS-K） were reported, respectively.Along with the development of CL technology, we get a full-scale understanding about the CL. As an important analytical method, CL has the merits of great sensitivity, wide dynamic range, simple equipment and easy automatization. However, the disadvantage of poor selectivity limited its application in many areas. So, the combination between HPLC and CL became a necessary consideration. Compounds were separated on the HPLC column and next mixed with CL reaction reagents, the lights emissed from the substances involved in this reaction course were recorded and conducted. Thus, the frame of HPLC-CL came into being. This analytical method has both excellences of CL and HPLC, at the same time, succeed in conquering the disadvantage of CL. Compare to some familiar detectors used in HPLC, such as UV detector, CL detector could achieve higher sensitivity for determination of many substances.Since the first report of HPLC-CL technique by Hartkopf, et al in 1974, this technique has developed rapidly. It has become a powerful tool for analysis of trace and ultra-trace ingredients and was widely used in the fields of metallurgy, chemical industry, pharmacy, environment, life science, biology and clinical medical science. The following four reports are our researching results.1. Determination of sinomenine hydrochloride by Reversed-Phase High Performance Liquid Chromatography with Chemiluminescence DetectionAn analytical method consisting of HPLC separation and chemiluminescence detection for determination of sinomenine hydrochloride（SIN） is described. It is based on the chemiluminescence reaction of KMnO₄-Na₂S₂O₃-SIN. The chemiluminescence更多还原