Fan Cai-ling, Xie Pu-hui, Cui Shu-min, Yang Li-na, Sun Qing, Ai Zhi-lu
Guang Pu Xue Yu Guang Pu Fen Xi. 2015 May;35(5):1300-5.
Recently, the problem of food security is more and more serious, and people pay attention to mercury because of the toxic of it. A new approach for the determination of mercury content in foodstuff is devised. In this paper, first, we design and synthesis a new kind of fluorescent probe whose matrix based on rhodamine B, hydrazine hydrate and hydroxy benzaldehyde. Through the analysis of H-NMR spectra of the synthesized product L1, we confirm that the synthetic substance is the adjacent carboxyl benzaldehyde hydrazone structure generation of rhodamine B. Then, we measure the fluorescence signal intensity of the probe with different concentrations of mercury ions fully upon complexation by fluorescence spectrometer and we can study the relationship between the mercury ion concentration and the fluorescence intensity and draw the standard working curve. Following, It's time to discuss the microwave digestion processing of tea, after digestion we use the synthetic probe Li for determination of mercury content in tea. The experimental results show that the maximum excitation wavelength of the probe and coordination compound are 568. 05 and 560. 00 nm, the maximum emission wavelength are 587. 94 and 580. 00 nm. Then we can find the best testing conditions to improve the degree of accuracy, that is: room temperature, 50% the methanol solution, 3. 0 mL pH 4. 0 buffer solution, in the extent of 30 min. The experimental results show that Na+, K+, Ca2+, Cu2+, Zn2+, Al3+ have little impact on the fluorescence intensity of the:probe. Fe3+, Mg2+, Ba2+ has a weak enhancement to the fluorescence intensity of the probe. While a low concentrations of Hg2+ have an obviously enhanced effect on the fluorescence intensity of the probe. In contrast to other metal ions, the probe for Hg2+ has a good selectivity. Linear relationship between the magnitude of increase in fluorescence intensity and concentration of mercury ion was in the range of 5~20 ng . L-1 with detection limit (3S/N) of 1. 9 ng . L-1. The proposed method was applied to determination of mercury ion in samples of tea and sausage and the obtained result and sample recovery were all satisfactory. The methods of analysis instrument has the advantages of simple structure, sensitivity, high accuracy, good selectivity and less volume of simple, without the need for enrichment, being very practical.
近年来,食品安全问题日益严重,人们因汞的毒性而对其予以关注。为此设计了一种测定食品中汞含量的新方法。本文首先设计并合成了一种新型荧光探针,其母体基于罗丹明B、水合肼和羟基苯甲醛。通过对合成产物L1的H-NMR谱图分析,确认合成物质为罗丹明B的邻羧基苯甲醛腙结构产物。然后,用荧光光谱仪测定不同汞离子浓度下探针络合后的荧光信号强度,研究汞离子浓度与荧光强度的关系并绘制标准工作曲线。接下来,对茶叶进行微波消解处理,消解后用合成探针L1测定茶叶中的汞含量。实验结果表明,探针及配合物的最大激发波长分别为568.05和560.00nm,最大发射波长分别为587.94和580.00nm。进而找出最佳测试条件以提高准确度,即:室温、50%甲醇溶液、3.0mL pH4.0缓冲溶液、30min。实验结果表明,Na+、K+、Ca2+、Cu2+、Zn2+、Al3+对探针荧光强度影响较小;Fe3+、Mg2+、Ba2+对探针荧光强度有微弱增强作用;而低浓度Hg2+对探针荧光强度有明显增强作用。与其他金属离子相比,该探针对Hg2+具有良好的选择性。荧光强度增加量与汞离子浓度在5~20ng·L-1范围内呈线性关系,检出限(3S/N)为1.9ng·L-1。该方法应用于茶叶和香肠样品中汞离子的测定,所得结果及样品回收率均令人满意。该分析仪器方法具有结构简单、灵敏度高、准确度好、选择性好、进样量少、无需富集等优点,实用性很强。