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目的基于衍生化-表面增强拉曼光谱技术,开展奶粉中亚硝酸盐快速定量分析方法的研究,建立一种简单、快速、灵敏的奶粉中亚硝酸盐的检测方法。方法采用重氮化-偶合反应,以金纳米粒子为增强试剂,将弱拉曼活性的亚硝酸根衍生成具有强拉曼活性的偶氮染料,通过对偶氮染料的测定实现对奶粉中亚硝酸盐的间接检测,优化了衍生化、前处理及检测条件。结果在优化条件下,方法的线性范围为0.030~1.0 mg/L、RSD小于14.8%、检出限为0.014 mg/L。方法用于奶粉样品分析的回收率为99.6%~128.9%、RSD为4.6%~15.8%。结论该方法简单快速、准确可靠,适用于乳制品中亚硝酸盐的分析检测。
OBJECTIVE To develop a simple, rapid and sensitive method for the detection of nitrite in milk powder based on the derivatization-surface enhanced Raman spectroscopy to develop a rapid and quantitative method for the determination of nitrite in milk powder. Methods The diazotization - coupling reaction was used to derivatize the weak Raman - active nitrite into the azo dye with strong Raman activity by using gold nanoparticle as reinforcement reagent. Indirect salt detection optimizes derivatization, pretreatment and detection conditions. Results Under the optimized conditions, the linear range of the method was 0.030-1.0 mg / L, the RSD was less than 14.8% and the limit of detection was 0.014 mg / L. The recoveries of the method for the analysis of milk powder samples ranged from 99.6% to 128.9% with a RSD of 4.6% to 15.8%. Conclusion The method is simple and rapid, accurate and reliable, suitable for the analysis and detection of nitrite in dairy products.