亚甲蓝和天青A与AuCl4^-离子缔合物的溶剂萃取导数-同步荧光光度法同时测定

Solvent Extraction & Derivative-synchronous Fluorescence Spectrometry on Simultaneous Determination of Methylene Blue and Azure A in Ion-association Complex Form with AuCl_4^-

在酸性介质中,亚甲蓝(MB)和天青A(AA)与AuCl4-形成离子缔合物,被1,2-二氯乙烷萃取后,以Δλ=20nm进行同步荧光扫描并采用一阶导数处理,2个缔合物分别在683和608nm附近出现峰值并能很好分开,且荧光强度分别与MB或AA浓度呈良好的线性关系,可用于2种吩噻嗪衍生物亚甲蓝和天青A的同时测定,检出限分别为7.9×10-9和1.78×10-8g/mL,其线性范围分别为3.0×10-8～4.8×10-6和6.0×10-8～5.8×10-6g/mL。研究了离子缔合物的组成和光谱特征,适宜的反应条件及影响因素。用于尿样和azureⅡ中亚甲蓝和天青A的同时测定,结果令人满意。

A synchronous fluorescence spectrometry combined with first order derivative treatment was developed for the simultaneous determination of methylene blue （MB） and azure A （AA）. The method is based upon the formation of ion-association complexes of AuCl4^- with MB and AA, and the solvent extraction of two complexes by 1,2-dichloroethane in an aeiditive medium. When [ MB ] [ AuCl4 ] 3 and [ AA ] [ AuCl4 ] 2 complexes were synchronously scanned at AA = 20 nm and treated with first order derivative techniques in organic phase, the derivative-synchronous fluorescence peaks appeared at 683 nm for [ MB] [ AuCI4 33 and at 608 nm for [ AA ] [ AuCl4 ] 2, respectively. The fluorescence intensities were directly proportional to the concentrations of MB at 683 nm and AA at 608 nm within a certain range. So, a simple, sensitive method has been developed for the simultaneous determination of MB and AA. The detection limit （3σ） and linear range were 7.90 × 10^-9 g/mL and 3.0× 10^-8 -4. 80 × 10^-6 g/mL for MB, 1.78 × 10^-8 g/mL and 6. 0 × 10^-8 - 5. 80 ×10^-6 g/mL for AA, respectively. In this work, the spectral characteristics and compostion of ionassociation complexes, the optimum conditions and the influences on the reaction system were investigated. The method can be applied to the simultaneous determination of AA and MB in urine samples and in Azure II with satisfactory results.