基于Ag(Ⅲ)配合物的流动注射-化学发光法快速测定血清中的氢化可的松

A Flow Injection Chemiluminescence Method for Determination of Hydrocortisone in Human Serum by Trivalent Silver Complex

基于氢化可的松对AgAg（Ⅲ）配合物-H2SO4体系化学发光信号的增敏作用,建立了一种测定血清中氢化可的松的流动注射-化学发光分析方法。当H2SO4浓度为1.0 mol/L,AgAg（Ⅲ）配合物浓度为2.5×10!4mol/L,流速为4.20 m L/min时,体系具有最强的化学发光。在最优实验条件下,相对发光强度与氢化可的松浓度在3.0×10!10~1.0×10!7g/m L范围内呈良好的线性关系,方法的检出限为2.2×10!10g/m L（3σ）。对5.0×10!8g/m L氢化可的松连续平行测定11次,其相对标准偏差为0.6%。本方法成功地用于人血清中氢化可的松的含量测定,回收率为93.0%~110.0%,相对标准偏差在0.3%~3.2%之间。通过研究该体系的紫外可见吸收光谱和荧光发射光谱,探讨了可能的化学发光机理。

A flow-injection chemiluminescence （FI-CL） reaction system with diperiodatoargentate（Ⅲ） wasdeveloped for the determination of hydrocortisone in human serum. The weak chemiluminescence signal from the reaction between DPA and sulfuric acid system can be greatly enhanced in the presence of hydrocortisone. The optimal conditions of the CL system were 1.0 mol/L H2SO4, 2.5 × 10^-4 mol/L diperiodatoargentate（Ⅲ）, and flow rate of 4. 20 mL/min. Under the optimal conditions, the CL intensity was linearly to the concentration of hydrocortisone from 3.0 × 10^-10 g/mL to 1.0× 10^-7 g/mL and the detection limit was 2.2 ×10^-10g/mL （3σ）. The relative standard deviation （RSD） was 0. 6% （n= 11） for 5. 0×10^-8 g/mL hydrocortisone solution. The proposed method was successfully applied to the direct determination of hydrocortisone in serum samples with the recoveries of 93.0%-110.0%, and the relative standard deviations were 0.3%-3.2%. The possible chemiluminescence mechanism was investigated by measuring fluorescence spectra and UV-vis absorption spectra of the system.