摘要
建立表面增强拉曼光谱法定性定量检测保健食品中非法添加物硝苯地平。采用柠檬酸三钠法制备胶体金,探索最优金胶浓度及粒径范围,确定以100 mL纯水中加入3 mL 1%氯金酸溶液及2.7 mL 1%柠檬酸三钠制备的金胶具备良好的信号增强效果,经粒径仪结果显示金溶胶粒在85 nm左右。利用拉曼光谱的特异性进行硝苯地平定性检测,结果发现部分降血压药物在(1334±3)cm^(-1)和(1642±3)cm^(-1)处有明显特征峰,用三聚氰胺作为内标物进行硝苯地平定量检测,以硝苯地平特征峰1334 cm^(-1)与三聚氰胺特征峰707 cm^(-1)的峰高比为纵坐标,硝苯地平浓度为横坐标进行线性拟合,结果发现硝苯地平质量浓度在0~100 mg/L有良好线性关系,相关系数为R^(2)=0.9957,定性检测线为5 mg/L,其固体、液体样品加标回收率分别为88.8%~96.5%和90.2%~96.6%,标准偏差分别为4.17%和3.49%。试验方法准确、灵敏、快速,可用于保健品中非法添加硝苯地平药物的定性定量检测。
Establish a qualitative and quantitative method for the determination of blood pressure lowering drugs in health food by portable laser Raman spectrometry.The SERS colloidal gold was prepared by trisodium citrate method.To explore the optimal concentration and particle size range of colloidal gold,the colloidal gold prepared by adding 3 mL 1%chlorauric acid solution and 2.7 mL 1%Trisodium citrate into 100 mL pure water had a good signal enhancement effect.The results of nanoparticle size analyzer showed that the diameter of colloidal gold was about 85 nm.The detection of blood pressure lowering drugs by portable laser Raman spectrometry showed that some blood pressure lowering drugs had obvious characteristic peaks at(1334±3)cm^(-1) and(1642±3)cm^(-1).The specificity of Raman spectrum was used for the qualitative determination of nifedipine.Melamine was used as internal standard to detect the content of nifedipine.The peak height ratio of nifedipine characteristic peak and melamine characteristic had a good linear relation with the concentration of nifedipine.The linear fitting correlation coefficient was 0.9957.The qualitative detection limit was 5 mg/L.The standard recoveries of solid and liquid samples were 88.8%-96.5%and 90.2%-96.6%,and the relative standard deviation were 4.17%and 3.49%.The method was accurate,sensitive and rapid,and could be used for the qualitative and quantitative detection of illegally added decompression drugs in health products.
作者
皮江一
周陶鸿
林津
彭青枝
PI Jiangyi;ZHOU Taohong;LIN Jin;PENG Qingzhi(Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075;Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-Derived Food for State Market Regulation,Wuhan 430075;Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Wuhan 430075)
出处
《食品工业》
CAS
2024年第1期264-268,共5页
The Food Industry
基金
湖北省重点研发项目(2020BCA091)。
