鲁米诺化学发光分析在药物分析中探究

鲁米诺化学发光分析在药物分析中的研究

化学教育 2000级3班梁斐

指导老师：张成孝教授

摘要:化学发光分析法是根据化学反应产生的光辐射的强度来确定物质含量的分析方法。该分析方法具有灵敏度高、线性范围宽、仪器简单、分析速度快、容易实现自动化等优点，受到人们的广泛关注。本论文利用鲁米诺体系流动注射化学发光法，建立了双嘧达莫和异烟肼的化学发光分析法。

我们在实验中发现，将含氮杂环的嘧啶类合成药物双嘧达莫溶液注入鲁米诺与铁氰化钾化学发光反应结束后的混合溶液中可产生强的化学发光信号。根据此实验现象并结合流动注射分析技术，建立了测定双嘧达莫的化学发光分析法。在优化的实验条件下，化学发光分析信号与双嘧达莫的浓度在1×10-10 ~ 4×10-7g/mL 之间呈良好的线性关系。根据IUPAC规定，计算得该方法的检出限为6×10-11g/mL。对1×10-8g/mL的双嘧达莫进行7次平行测量，相对标准偏差为1.1%。该方法用于双嘧达莫片剂中双嘧达莫含量的测定，并与药典中标准方法进行对照，没有显著性差异。

实验发现将异烟肼溶液注入鲁米诺与高锰酸钾化学发光反应结束后的混合溶液中可产生强的化学发光信号。根据此实验现象并结合流动注射分析技术，建立了测定异烟肼的化学发光分析法。在优化的实验条件下，化学发光分析信号与异烟肼的浓度在5×10-8 ~ 1×10-4g/mL之间呈良好的线性关系。根据IUPAC规定，计算得该方法的检出限为1×10-8g/mL 。对1×10-6g/mL的异烟肼进行7次平行测量，相对标准偏差为1.1%。该方法用于异烟肼片剂中异烟肼含量的测定，结果令人满意。

关键词：流动注射分析化学发光反应鲁米诺双嘧达莫异烟肼

The analytical application of luminol chemiluminescence in

Pharmaceutical assay

Liang Fei ZhangChengxiao professor

Abstract：Chemiluminescence (CL) analysis promises high sensitivity with simple instrumentation (no monochromator required) and rapidly in signal detection (normally 0.1-10s). When coupled with flow injection analysis (FIA), CL-based FIA methods provide cheap, rapid, simple and reproducible means of detection and therefore, it has been extensively used in many fields, such as biological, clinical, environmental.

When dipyridamole(DIP) was injected into the reaction mixture after the finish of the reaction between luminol and K3Fe(CN)6, a new CL reaction was initiated to produce strong CL emission. Based on this phenomenon, a novel CL system for DIP combined with flow injection analysis was presented in this paper. The CL intensity responded linearly to the concentration of DIP in the range of 1×10-10 ~ 4×10-7 g/mL with a detection limit of 6×10-11g/mL. The relative standard deviation was 1.1% for 1×10-8 g/mL DIP solution( n=7). The method has been applied to determine DIP in tablets and the results are in agreement with traditional method using UV spectrometry.

It was found that a strong CL signal was produced when isoniazid was injected into the reaction mixture after the finish of the reaction between luminol and KMnO4. Based on this finding, a simple flow injection CL method was established for determination of isoniazid. Under the optimized condition, the CL signals responded linearly to the concentration of isoniazid from 5×10-8 g/mL to 1×10-4g/mL with the detection limit of 1×10-8 g/mL isoniazid. The relative standard deviation was 1.1% for 1×10-6 g/mL isoniazid (n=7). This method developed has been applied to determine isoniazid in tablets with satisfactory results.

Keywords: Flow-injection analysis; Chemiluminescence reaction; Luminol; Dipyridamole；Isoniazid