Murillo Pulgarín José A, García Bermejo Luisa F, Lemus Gallego José M, Sánchez García M Nieves
Department of Analytical Chemistry and Foods Technology, University of Castilla-La Mancha, 13071 Ciudad Real, Spain.
Talanta. 2008 Feb 15;74(5):1539-46. doi: 10.1016/j.talanta.2007.09.032. Epub 2007 Oct 2.
The first application of the flow analysis coupled with chemiluminescence detection and based on stopped-flow chemistry to the simultaneous determination of two components, using a two equation system, is described. The proposed method to determine simultaneously morphine and naloxone is based on the chemiluminescence oxidation of these compounds by their reaction with potassium permanganate in an acidic medium. The main feature of the system used is that the recording of the whole chemiluminescence intensity-versus-time profiles can be obtained, using the stopped-flow technique in a continuous-flow system. Then, the chemiluminescent signals obtained at two times of these profiles can be used to determine the concentration of both opiate narcotics. The effect of common emission enhancers on the chemiluminescence emission of these compounds in different acidic media, using the above-mentioned technique, was studied, in order to achieve the best conditions in which, the CL profiles of both compounds should be additive. The parameters selected were sulphuric acid 1.0 mol L(-1), permanganate 0.2 mmolL(-1) and formaldehyde 0.8 mol L(-1). Taken in account the different profiles of the transient CL signal obtained with each compounds, using the selected chemical conditions, two measurement times (1.4 and 4.8s) of these responses curves were considered with the purpose to establish a simple 2 x 2 matrix calculation. Using the chemiluminiscent signals obtained at these times, a linear calibration graph was obtained for each one of the compounds between 0.01 and 1.00 mg L(-1) for morphine and 0.10-1.50 mg L(-1) for naloxone. The present chemiluminescence procedure was applied to the determination of both compounds in mixtures and was found to be satisfactory.
描述了流动分析与化学发光检测相结合并基于停流化学，使用二元方程组同时测定两种组分的首次应用。所提出的同时测定吗啡和纳洛酮的方法基于这些化合物在酸性介质中与高锰酸钾反应的化学发光氧化。所用系统的主要特点是，在连续流动系统中使用停流技术，可以获得整个化学发光强度随时间变化的曲线记录。然后，利用这些曲线在两个时刻获得的化学发光信号来测定两种阿片类麻醉剂的浓度。使用上述技术，研究了常见发射增强剂在不同酸性介质中对这些化合物化学发光发射的影响，以实现最佳条件，使两种化合物的化学发光曲线具有加和性。选择的参数为硫酸1.0 mol L(-1)、高锰酸钾0.2 mmolL(-1)和甲醛0.8 mol L(-1)。考虑到在选定化学条件下每种化合物获得的瞬态化学发光信号的不同曲线，为了建立简单的2×2矩阵计算，考虑了这些响应曲线的两个测量时间（1.4和4.8秒）。利用在这些时间获得的化学发光信号，得到了每种化合物的线性校准曲线，吗啡在0.01至1.00 mg L(-1)之间，纳洛酮在0.10 - 1.50 mg L(-1)之间。将本化学发光方法应用于混合物中两种化合物的测定，结果令人满意。
