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目的:建立一种高灵敏度的共振荧光光谱法测定奶粉中三聚氰胺的新方法。方法:对B-R缓冲溶液-CPC表面活性剂介质中的甲酚紫高氯酸盐进行同步扫描,应用三维荧光和吸收光谱分析同步扫描光谱峰的共振荧光特性;基于三聚氰胺对甲酚紫高氯酸盐的共振荧光强度的抑制作用,建立阻抑共振荧光测定三聚氰胺的分析方法。结果:在9.6×10-8～2.8×10-6mol/L浓度范围内,体系的△F值与三聚氰胺浓度(c,10-6mol/L)之间具有良好的线性关系,线性回归方程为△F=106.59c-5.44,相关系数r=0.9993。检出限为2.87×10-8mol/L。奶粉样品测定的相对标准偏差为1.9%～2.7%,加标回收率为95.0%～103.1%。结论:方法灵敏,操作简便,分析成本低,用于奶粉中三聚氰胺的测定,结果满意。
Objective: To establish a new method of high sensitivity resonance fluorescence spectrometry for the determination of melamine in milk powder. METHODS: The cresyl violet perchlorate in BR buffer solution-CPC surfactant medium was scanned synchronously. The three-dimensional fluorescence and absorption spectra were used to analyze the resonance fluorescence characteristics of the peak of synchronous scanning. Based on the results of melamine- Salt resonance fluorescence intensity inhibition, inhibition of resonance fluorescence determination of melamine method of analysis. Results: In the concentration range of 9.6 × 10-8 ~ 2.8 × 10-6mol / L, there was a good linear relationship between △ F value and melamine concentration (c, 10-6mol / L), the linear regression equation was △ F = 106.59c-5.44, correlation coefficient r = 0.9993. The detection limit was 2.87 × 10-8mol / L. The relative standard deviations (RSDs) of milk powder samples were 1.9% ~ 2.7% and the recoveries were 95.0% ~ 103.1%. Conclusion: The method is sensitive, simple and easy to operate, low in analysis cost and is used in the determination of melamine in milk powder with satisfactory results.