Pacheco Wagner F, Batalha João A L, de Oliveira Cláudia C, Aucelio Ricardo Q
Chemistry Department, Pontifícia Universidade Católica do Rio de Janeiro (PUC-RJ), Rio de Janeiro, RJ 22453-900, Brazil.
Talanta. 2008 Feb 15;74(5):1442-9. doi: 10.1016/j.talanta.2007.09.022. Epub 2007 Oct 2.
In this work, a fluorimetric approach for the determination of cyclofenil, 4-4'-(cyclohexylidenemethylene)bis(phenylacetate), is presented. The method was based on the intense fluorescence (250/410 nm) observed after a UV photochemical treatment of cyclofenil. The influence of the pH and solvent system and UV exposure time on the fluorescence magnitude was studied. Optimization of parameters was made using experimental design (factorial design and central composite design). Limit of detection (3S(b)/m) were estimated to be 1.1 x 10(-8)mol L(-1) with the linear dynamic range extending up to 8 x 10(-5)mol L(-1). This analytical approach was tested through the analysis of a commercial pharmaceutical formulation. In this case, tests enabled an average recovery of 98.3+/-3.9% (for n=9) using the analytical curve. The identification of the fluorescent derivative is proposed based on results achieved from GC-MS.
本研究提出了一种荧光分析法用于测定环苯吩嗪(4-4'-(环己基亚甲基)双(苯乙酸酯))。该方法基于环苯吩嗪经紫外光化学处理后观察到的强烈荧光(250/410 nm)。研究了pH值、溶剂体系和紫外照射时间对荧光强度的影响。使用实验设计(析因设计和中心复合设计)对参数进行了优化。检测限(3S(b)/m)估计为1.1×10⁻⁸ mol L⁻¹,线性动态范围扩展至8×10⁻⁵ mol L⁻¹。通过对市售药物制剂的分析对该分析方法进行了测试。在这种情况下,使用分析曲线进行测试,平均回收率为98.3±3.9%(n = 9)。基于气相色谱-质谱联用(GC-MS)的结果对荧光衍生物进行了鉴定。