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机构地区:[1]中山大学化学与化学工程学院,广州510275
出 处:《分析化学》2015年第8期1218-1223,共6页Chinese Journal of Analytical Chemistry
基 金:国家重大科学仪器设备开发专项(No.2011YQ03012409);国家自然科学基金项目(Nos.21277176;21275168;21127008)~~
摘 要:建立了食品中香豆素的表面增强拉曼光谱定量分析法。以粒径约为55 nm的金纳米粒子为拉曼活性基底,以p H=5.0 HCl-KCl溶液为溶剂,釆用便携式拉曼仪进行分析。通过实验优化得到最佳测定条件(金纳米溶胶浓缩倍数为50倍,激光照射时间为5 s,金纳米溶胶与溶液的混合比例为1∶1),建立了食品中游离香豆素直接检测方法,方法在1.0~100.0 mg/L的浓度范围内具有良好的线性,检出限为0.91 mg/L。将建立的分析方法用于蔬果、糖果、糕点等实际样品中香豆素的检测(样品前处理过程:称取10 g样品于烧杯中,加入50 m L溶剂,超声提取0.5 h后,定容至100 m L,摇匀后过滤,取10 m L定容至100 m L,摇匀得到样品处理液),香豆素含量在0.61~5.52 g/kg之间;样品的加标回收率为75.12%~103.2%,相对标准偏差为0.6%~14%。结果表明,本方法快速准确、操作简单,可用于水果、糖果、糕点中香豆素的快速检测。A method was established for the determination of coumarin in various foods by surface-enhanced Raman spectroscopy in a hydrochloric acid-potassium chloride solution( p H = 5. 0) with 55 nm Au nanoparticles as Raman substrate. Under the optimal experiment conditions such as concentrated gold sol with concentration multiple of 50,5 s of laser irradiation time and 1 ∶ 1 mixing ratio of gold sol and solution,the method was used for the direct determination of coumarin. The method had a good linearity between the peak intensity and the courmain concentration in the range of 1. 00- 100. 0 mg / L,and the detection limit was0. 91 mg / L. For the determination of real samples of courmain in vegetables,fruits,sweets and pastries,10 g of sample was added in 50 m L of hydrochloric acid-potassium chloride solution in a beaker,and then ultrasonically extracted for 0. 5 h. After transferred into a 100-m L flask,the sample solution was filtered and10 m L of supernatant was taken and diluted to 100 m L for the further analysis. The concentration of courmain was determined to be 0. 61-5. 52 g / kg. The relative standard deviations were 0. 6%-14. 0%. The spiked recoveries of these samples ranged from 75. 1% to 103. 2%. This method is simple,and has wide linear range and high accuracy.
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